# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
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# Please retain this information to preserve the provenance of
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data_cocl2mic2
_database_code_depnum_ccdc_archive 'CCDC 1959508'
loop_
_audit_author_name
_audit_author_address
'Milan Gembicky'
;University of California, San Diego
United States of America
;
_audit_update_record
;
2019-10-18 deposited with the CCDC. 2020-02-06 downloaded from the CCDC.
;
_audit_creation_date 2019-10-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic
'(1,3-bis(2,6-diisopropylphenyl)-5-phenyl-2,3-dihydro-1H-1,2,3-triazol-4-yl)(1-(2,6-diisopropylphenyl)-3-(2-ethyl-6-isopropylphenyl)-5-phenyl-2,3-dihydro-1H-1,2,3-triazol-4-yl)cobalt(II) chloride'
_chemical_formula_moiety 'C64 H78 Cl2 Co N6'
_chemical_formula_sum 'C64 H78 Cl2 Co N6'
_chemical_formula_weight 1061.15
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 13.6433(10)
_cell_length_b 15.2982(11)
_cell_length_c 15.8757(12)
_cell_angle_alpha 97.413(2)
_cell_angle_beta 91.715(3)
_cell_angle_gamma 97.494(2)
_cell_volume 3254.1(4)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 8967
_cell_measurement_temperature 100
_cell_measurement_theta_max 43.400
_cell_measurement_theta_min 4.702
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.385
_exptl_absorpt_correction_T_max 0.7453
_exptl_absorpt_correction_T_min 0.7165
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0633 before and 0.0600 after correction.
The Ratio of minimum to maximum transmission is 0.9516.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'dull blue'
_exptl_crystal_colour_lustre dull
_exptl_crystal_colour_primary blue
_exptl_crystal_density_diffrn 1.083
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1130
_exptl_crystal_preparation
'Two equivalents of free carbene with 1 eq of CoCl2 in THF'
_exptl_crystal_recrystallization_method 'Pentane into toluene'
_exptl_crystal_size_max 0.05
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.03
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0837
_diffrn_reflns_av_unetI/netI 0.0699
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 83104
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.413
_diffrn_reflns_theta_min 1.885
_diffrn_ambient_temperature 100.0
_diffrn_detector 'Bruker APEX CCD'
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type 'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device 'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type ?
_diffrn_measurement_method ?
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe X-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'sealed tube'
_diffrn_source_type fine-focus
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 8931
_reflns_number_total 13291
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement ?
_computing_data_collection 'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XT (Sheldrick, 2008)'
_refine_diff_density_max 0.786
_refine_diff_density_min -0.269
_refine_diff_density_rms 0.055
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 674
_refine_ls_number_reflns 13291
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0811
_refine_ls_R_factor_gt 0.0448
_refine_ls_restrained_S_all 1.036
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.3007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0946
_refine_ls_wR_factor_ref 0.1063
_refine_special_details SQUEEZE
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C38(H38), C62(H62), C35(H35), C47(H47), C26(H26), C59(H59), C50(H50), C23(H23)
2.b Aromatic/amide H refined with riding coordinates:
C10(H10), C6(H6), C16(H16), C8(H8), C9(H9), C55(H55), C12(H12), C7(H7),
C15(H15), C56(H56), C31(H31), C14(H14), C13(H13), C33(H33), C32(H32), C57(H57),
C19(H19), C45(H45), C21(H21), C43(H43), C20(H20), C44(H44)
2.c Idealised Me refined as rotating group:
C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C63(H63A,H63B,H63C), C51(H51A,H51B,
H51C), C52(H52A,H52B,H52C), C25(H25A,H25B,H25C), C40(H40A,H40B,H40C), C37(H37A,
H37B,H37C), C64(H64A,H64B,H64C), C61(H61A,H61B,H61C), C27(H27A,H27B,H27C),
C28(H28A,H28B,H28C), C49(H49A,H49B,H49C), C48(H48A,H48B,H48C), C60(H60A,H60B,
H60C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.25188(2) 0.66739(2) 0.64764(2) 0.01800(9) Uani 1 1 d . . . . .
Cl1 Cl 0.31285(4) 0.54660(3) 0.58322(4) 0.02712(14) Uani 1 1 d . . . . .
Cl2 Cl 0.12321(4) 0.71258(4) 0.58054(4) 0.03119(15) Uani 1 1 d . . . . .
N6 N 0.45645(13) 0.90677(11) 0.68810(11) 0.0200(4) Uani 1 1 d . . . . .
N5 N 0.48544(13) 0.87418(11) 0.61251(11) 0.0206(4) Uani 1 1 d . . . . .
N4 N 0.42558(12) 0.79661(10) 0.59490(11) 0.0173(4) Uani 1 1 d . . . . .
N3 N 0.20100(13) 0.57819(11) 0.88834(11) 0.0206(4) Uani 1 1 d . . . . .
N1 N 0.11981(13) 0.57657(11) 0.77469(11) 0.0211(4) Uani 1 1 d . . . . .
N2 N 0.11273(13) 0.54756(12) 0.85028(11) 0.0237(4) Uani 1 1 d . . . . .
C3 C 0.35944(15) 0.77650(13) 0.65540(13) 0.0170(5) Uani 1 1 d . . . . .
C5 C 0.36413(16) 0.66341(13) 0.86417(13) 0.0195(5) Uani 1 1 d . . . . .
C2 C 0.26126(15) 0.62567(13) 0.83729(13) 0.0174(5) Uani 1 1 d . . . . .
C1 C 0.20897(15) 0.62508(13) 0.76070(13) 0.0184(5) Uani 1 1 d . . . . .
C4 C 0.38174(15) 0.85120(13) 0.71695(13) 0.0188(5) Uani 1 1 d . . . . .
C29 C 0.44010(16) 0.74268(13) 0.51467(13) 0.0196(5) Uani 1 1 d . . . . .
C11 C 0.33517(16) 0.87254(13) 0.79847(14) 0.0212(5) Uani 1 1 d . . . . .
C10 C 0.38958(17) 0.70687(14) 0.94631(14) 0.0237(5) Uani 1 1 d . . . . .
H10 H 0.339663 0.713812 0.986158 0.028 Uiso 1 1 calc R . . . .
C34 C 0.51458(16) 0.68890(13) 0.51315(14) 0.0221(5) Uani 1 1 d . . . . .
C38 C 0.58261(16) 0.68568(14) 0.58976(14) 0.0238(5) Uani 1 1 d . . . . .
H38 H 0.556501 0.719839 0.640244 0.029 Uiso 1 1 calc R . . . .
C6 C 0.43849(16) 0.65521(14) 0.80584(14) 0.0234(5) Uani 1 1 d . . . . .
H6 H 0.422290 0.626217 0.749629 0.028 Uiso 1 1 calc R . . . .
C16 C 0.39043(17) 0.90957(14) 0.87274(14) 0.0248(5) Uani 1 1 d . . . . .
H16 H 0.460394 0.922201 0.871641 0.030 Uiso 1 1 calc R . . . .
C8 C 0.56026(17) 0.73083(15) 0.91213(15) 0.0284(6) Uani 1 1 d . . . . .
H8 H 0.627307 0.753028 0.928659 0.034 Uiso 1 1 calc R . . . .
C9 C 0.48748(17) 0.73994(15) 0.96990(15) 0.0285(6) Uani 1 1 d . . . . .
H9 H 0.504465 0.768946 1.025999 0.034 Uiso 1 1 calc R . . . .
C39 C 0.58597(18) 0.59095(14) 0.60891(15) 0.0287(6) Uani 1 1 d . . . . .
H39A H 0.518850 0.563080 0.617614 0.043 Uiso 1 1 calc GR . . . .
H39B H 0.627846 0.592324 0.660431 0.043 Uiso 1 1 calc GR . . . .
H39C H 0.613373 0.556560 0.560986 0.043 Uiso 1 1 calc GR . . . .
C55 C 0.4910(2) 1.14885(15) 0.76418(15) 0.0346(6) Uani 1 1 d . . . . .
H55 H 0.456313 1.198791 0.764070 0.041 Uiso 1 1 calc R . . . .
C17 C 0.03173(16) 0.55223(15) 0.71734(14) 0.0252(5) Uani 1 1 d . . . . .
C62 C 0.65870(18) 0.92751(15) 0.76256(15) 0.0304(6) Uani 1 1 d . . . . .
H62 H 0.614955 0.870940 0.740841 0.036 Uiso 1 1 calc R . . . .
C58 C 0.59707(18) 1.00329(14) 0.76475(14) 0.0264(5) Uani 1 1 d . . . . .
C12 C 0.23282(17) 0.85326(14) 0.80124(15) 0.0287(6) Uani 1 1 d . . . . .
H12 H 0.194376 0.827526 0.751160 0.034 Uiso 1 1 calc R . . . .
C53 C 0.50202(18) 0.99484(13) 0.72672(14) 0.0244(5) Uani 1 1 d . . . . .
C7 C 0.53571(17) 0.68945(15) 0.83028(15) 0.0277(5) Uani 1 1 d . . . . .
H7 H 0.585889 0.684434 0.790409 0.033 Uiso 1 1 calc R . . . .
C15 C 0.34398(18) 0.92809(15) 0.94820(15) 0.0318(6) Uani 1 1 d . . . . .
H15 H 0.382073 0.953953 0.998420 0.038 Uiso 1 1 calc R . . . .
C18 C -0.04078(18) 0.60811(16) 0.72221(16) 0.0338(6) Uani 1 1 d . . . . .
C56 C 0.5832(2) 1.15939(15) 0.80409(15) 0.0339(6) Uani 1 1 d . . . . .
H56 H 0.611223 1.216313 0.831859 0.041 Uiso 1 1 calc R . . . .
C31 C 0.39219(19) 0.69447(15) 0.36988(15) 0.0327(6) Uani 1 1 d . . . . .
H31 H 0.350763 0.694933 0.320813 0.039 Uiso 1 1 calc R . . . .
C30 C 0.37709(17) 0.74820(14) 0.44464(14) 0.0233(5) Uani 1 1 d . . . . .
C14 C 0.24228(19) 0.90898(17) 0.95045(16) 0.0379(7) Uani 1 1 d . . . . .
H14 H 0.210451 0.921461 1.002200 0.045 Uiso 1 1 calc R . . . .
C22 C 0.02477(18) 0.47216(15) 0.66248(14) 0.0283(6) Uani 1 1 d . . . . .
C41 C 0.22374(17) 0.55380(14) 0.97146(14) 0.0251(5) Uani 1 1 d . . . . .
C13 C 0.18699(18) 0.87160(16) 0.87706(16) 0.0355(6) Uani 1 1 d . . . . .
H13 H 0.117123 0.858409 0.878666 0.043 Uiso 1 1 calc R . . . .
C33 C 0.52684(18) 0.63758(14) 0.43558(15) 0.0286(6) Uani 1 1 d . . . . .
H33 H 0.577570 0.600413 0.431310 0.034 Uiso 1 1 calc R . . . .
C36 C 0.3488(2) 0.90675(15) 0.44256(16) 0.0379(6) Uani 1 1 d . . . . .
H36A H 0.403601 0.923961 0.485261 0.057 Uiso 1 1 calc GR . . . .
H36B H 0.299571 0.947798 0.452299 0.057 Uiso 1 1 calc GR . . . .
H36C H 0.374030 0.909153 0.385637 0.057 Uiso 1 1 calc GR . . . .
C54 C 0.44723(18) 1.06534(14) 0.72351(15) 0.0282(6) Uani 1 1 d . . . . .
C32 C 0.4660(2) 0.64038(15) 0.36526(15) 0.0341(6) Uani 1 1 d . . . . .
H32 H 0.475006 0.604819 0.313157 0.041 Uiso 1 1 calc R . . . .
C57 C 0.63572(19) 1.08823(15) 0.80432(14) 0.0318(6) Uani 1 1 d . . . . .
H57 H 0.699610 1.097169 0.832027 0.038 Uiso 1 1 calc R . . . .
C35 C 0.30057(18) 0.81186(15) 0.44955(15) 0.0307(6) Uani 1 1 d . . . . .
H35 H 0.271512 0.812381 0.506670 0.037 Uiso 1 1 calc R . . . .
C42 C 0.18597(18) 0.59971(15) 1.04247(15) 0.0309(6) Uani 1 1 d . . . . .
C47 C 0.11763(19) 0.66906(15) 1.03443(16) 0.0351(6) Uani 1 1 d . . . . .
H47 H 0.125901 0.689271 0.977315 0.042 Uiso 1 1 calc R . . . .
C26 C 0.10192(19) 0.40913(15) 0.66293(15) 0.0331(6) Uani 1 1 d . . . . .
H26 H 0.166264 0.444444 0.685693 0.040 Uiso 1 1 calc R . . . .
C59 C 0.34718(19) 1.05719(15) 0.67680(17) 0.0370(6) Uani 1 1 d . . . . .
H59 H 0.328409 0.993425 0.652215 0.044 Uiso 1 1 calc R . . . .
C19 C -0.12513(19) 0.58155(18) 0.66869(17) 0.0429(7) Uani 1 1 d . . . . .
H19 H -0.176961 0.617538 0.670858 0.051 Uiso 1 1 calc R . . . .
C46 C 0.28301(18) 0.48649(15) 0.97487(15) 0.0298(6) Uani 1 1 d . . . . .
C50 C 0.31795(18) 0.43362(15) 0.89654(16) 0.0327(6) Uani 1 1 d . . . . .
H50 H 0.292957 0.457449 0.845423 0.039 Uiso 1 1 calc R . . . .
C45 C 0.3083(2) 0.46795(17) 1.05585(17) 0.0424(7) Uani 1 1 d . . . . .
H45 H 0.349981 0.423758 1.061719 0.051 Uiso 1 1 calc R . . . .
C23 C -0.03313(18) 0.69440(17) 0.78314(18) 0.0429(7) Uani 1 1 d . . . . .
H23 H 0.034380 0.705061 0.811910 0.051 Uiso 1 1 calc R . . . .
C21 C -0.0605(2) 0.45063(17) 0.60902(16) 0.0385(7) Uani 1 1 d . . . . .
H21 H -0.067476 0.397983 0.569195 0.046 Uiso 1 1 calc R . . . .
C63 C 0.7016(2) 0.91835(16) 0.84995(16) 0.0439(7) Uani 1 1 d . . . . .
H63A H 0.748571 0.971414 0.870710 0.066 Uiso 1 1 calc GR . . . .
H63B H 0.735944 0.865641 0.846058 0.066 Uiso 1 1 calc GR . . . .
H63C H 0.648083 0.912084 0.889424 0.066 Uiso 1 1 calc GR . . . .
C43 C 0.2129(2) 0.57635(18) 1.12150(16) 0.0458(8) Uani 1 1 d . . . . .
H43 H 0.188482 0.605037 1.171721 0.055 Uiso 1 1 calc R . . . .
C51 C 0.43082(19) 0.44321(17) 0.89531(17) 0.0427(7) Uani 1 1 d . . . . .
H51A H 0.457407 0.506183 0.897474 0.064 Uiso 1 1 calc GR . . . .
H51B H 0.450222 0.409768 0.843004 0.064 Uiso 1 1 calc GR . . . .
H51C H 0.457176 0.419836 0.944678 0.064 Uiso 1 1 calc GR . . . .
C20 C -0.1346(2) 0.50386(18) 0.61263(17) 0.0449(7) Uani 1 1 d . . . . .
H20 H -0.192451 0.487008 0.576375 0.054 Uiso 1 1 calc R . . . .
C52 C 0.2739(2) 0.33545(16) 0.89045(18) 0.0442(7) Uani 1 1 d . . . . .
H52A H 0.298082 0.310238 0.939531 0.066 Uiso 1 1 calc GR . . . .
H52B H 0.293805 0.302726 0.837970 0.066 Uiso 1 1 calc GR . . . .
H52C H 0.201505 0.330632 0.889971 0.066 Uiso 1 1 calc GR . . . .
C25 C -0.0458(2) 0.77424(18) 0.7379(2) 0.0558(9) Uani 1 1 d . . . . .
H25A H 0.002994 0.779014 0.694073 0.084 Uiso 1 1 calc GR . . . .
H25B H -0.035858 0.828466 0.779143 0.084 Uiso 1 1 calc GR . . . .
H25C H -0.112642 0.766717 0.711319 0.084 Uiso 1 1 calc GR . . . .
C40 C 0.6858(2) 0.73071(19) 0.5765(2) 0.0560(9) Uani 1 1 d . . . . .
H40A H 0.714897 0.695948 0.529899 0.084 Uiso 1 1 calc GR . . . .
H40B H 0.727098 0.734583 0.628790 0.084 Uiso 1 1 calc GR . . . .
H40C H 0.681896 0.790697 0.562393 0.084 Uiso 1 1 calc GR . . . .
C37 C 0.21537(19) 0.78470(18) 0.38210(17) 0.0447(7) Uani 1 1 d . . . . .
H37A H 0.240188 0.791662 0.325729 0.067 Uiso 1 1 calc GR . . . .
H37B H 0.163523 0.822658 0.394086 0.067 Uiso 1 1 calc GR . . . .
H37C H 0.187976 0.722425 0.383429 0.067 Uiso 1 1 calc GR . . . .
C64 C 0.7411(2) 0.94095(19) 0.70073(19) 0.0534(8) Uani 1 1 d . . . . .
H64A H 0.712036 0.941208 0.643587 0.080 Uiso 1 1 calc GR . . . .
H64B H 0.781556 0.892409 0.699857 0.080 Uiso 1 1 calc GR . . . .
H64C H 0.782733 0.997848 0.719041 0.080 Uiso 1 1 calc GR . . . .
C44 C 0.2738(2) 0.51277(19) 1.12754(17) 0.0522(8) Uani 1 1 d . . . . .
H44 H 0.292563 0.499320 1.182022 0.063 Uiso 1 1 calc R . . . .
C61 C 0.3525(2) 1.11289(17) 0.60291(19) 0.0561(9) Uani 1 1 d . . . . .
H61A H 0.366129 1.176195 0.625494 0.084 Uiso 1 1 calc GR . . . .
H61B H 0.289160 1.101385 0.569935 0.084 Uiso 1 1 calc GR . . . .
H61C H 0.405462 1.096680 0.566112 0.084 Uiso 1 1 calc GR . . . .
C27 C 0.0721(2) 0.33992(18) 0.72186(17) 0.0505(8) Uani 1 1 d . . . . .
H27A H 0.064255 0.370040 0.779109 0.076 Uiso 1 1 calc GR . . . .
H27B H 0.123538 0.301034 0.723989 0.076 Uiso 1 1 calc GR . . . .
H27C H 0.009330 0.304246 0.700332 0.076 Uiso 1 1 calc GR . . . .
C28 C 0.1176(2) 0.36158(18) 0.57474(16) 0.0484(8) Uani 1 1 d . . . . .
H28A H 0.057308 0.321573 0.553866 0.073 Uiso 1 1 calc GR . . . .
H28B H 0.172855 0.327004 0.578070 0.073 Uiso 1 1 calc GR . . . .
H28C H 0.132586 0.405630 0.535666 0.073 Uiso 1 1 calc GR . . . .
C49 C 0.1413(2) 0.75083(18) 1.10182(18) 0.0532(8) Uani 1 1 d . . . . .
H49A H 0.127345 0.733796 1.158123 0.080 Uiso 1 1 calc GR . . . .
H49B H 0.100369 0.796229 1.089755 0.080 Uiso 1 1 calc GR . . . .
H49C H 0.211404 0.774813 1.100745 0.080 Uiso 1 1 calc GR . . . .
C48 C 0.0090(2) 0.62761(18) 1.0387(2) 0.0548(9) Uani 1 1 d . . . . .
H48A H -0.007644 0.579589 0.991310 0.082 Uiso 1 1 calc GR . . . .
H48B H -0.034380 0.673317 1.034757 0.082 Uiso 1 1 calc GR . . . .
H48C H 0.000010 0.603566 1.092641 0.082 Uiso 1 1 calc GR . . . .
C60 C 0.2669(2) 1.08271(18) 0.7376(2) 0.0579(9) Uani 1 1 d . . . . .
H60A H 0.266112 1.047241 0.784812 0.087 Uiso 1 1 calc GR . . . .
H60B H 0.202236 1.071141 0.706833 0.087 Uiso 1 1 calc GR . . . .
H60C H 0.281305 1.146044 0.759922 0.087 Uiso 1 1 calc GR . . . .
C24 C -0.1084(3) 0.6873(3) 0.8515(2) 0.0908(13) Uani 1 1 d . . . . .
H24A H -0.175427 0.679483 0.825122 0.136 Uiso 1 1 calc GR . . . .
H24B H -0.098474 0.741792 0.892409 0.136 Uiso 1 1 calc GR . . . .
H24C H -0.099938 0.636146 0.880955 0.136 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.02016(17) 0.01604(16) 0.01750(16) -0.00050(12) 0.00123(12) 0.00399(12)
Cl1 0.0306(3) 0.0203(3) 0.0301(3) -0.0028(2) 0.0072(3) 0.0068(2)
Cl2 0.0277(3) 0.0309(3) 0.0347(3) 0.0021(3) -0.0076(3) 0.0073(3)
N6 0.0293(11) 0.0121(9) 0.0189(10) 0.0017(8) 0.0016(8) 0.0036(8)
N5 0.0281(11) 0.0145(9) 0.0189(10) 0.0013(8) 0.0013(8) 0.0022(8)
N4 0.0222(10) 0.0125(9) 0.0173(10) 0.0009(7) -0.0008(8) 0.0039(8)
N3 0.0224(10) 0.0195(9) 0.0185(10) -0.0007(8) 0.0042(8) 0.0003(8)
N1 0.0228(10) 0.0197(10) 0.0184(10) -0.0034(8) 0.0046(8) -0.0004(8)
N2 0.0249(11) 0.0230(10) 0.0204(10) -0.0033(8) 0.0046(8) -0.0017(8)
C3 0.0198(11) 0.0177(11) 0.0160(11) 0.0043(9) -0.0013(9) 0.0100(9)
C5 0.0229(12) 0.0163(11) 0.0194(12) 0.0053(9) 0.0003(10) 0.0003(9)
C2 0.0216(12) 0.0132(10) 0.0171(11) 0.0002(9) 0.0056(9) 0.0021(9)
C1 0.0181(12) 0.0144(11) 0.0208(12) -0.0051(9) 0.0041(9) 0.0012(9)
C4 0.0231(12) 0.0155(11) 0.0192(12) 0.0044(9) 0.0010(10) 0.0061(9)
C29 0.0288(13) 0.0131(11) 0.0159(11) 0.0007(9) 0.0059(10) -0.0010(9)
C11 0.0268(13) 0.0144(11) 0.0230(12) -0.0001(9) 0.0030(10) 0.0075(9)
C10 0.0276(13) 0.0218(12) 0.0211(12) 0.0028(10) 0.0033(10) 0.0004(10)
C34 0.0290(13) 0.0141(11) 0.0233(12) 0.0032(9) 0.0057(10) 0.0012(10)
C38 0.0258(13) 0.0200(12) 0.0256(13) -0.0008(10) 0.0020(10) 0.0070(10)
C6 0.0264(13) 0.0221(12) 0.0227(12) 0.0067(10) -0.0007(10) 0.0044(10)
C16 0.0259(13) 0.0234(12) 0.0252(13) 0.0009(10) 0.0010(10) 0.0058(10)
C8 0.0227(13) 0.0320(13) 0.0309(14) 0.0138(11) -0.0064(11) -0.0030(11)
C9 0.0329(14) 0.0269(13) 0.0230(13) 0.0041(10) -0.0057(11) -0.0047(11)
C39 0.0350(14) 0.0240(12) 0.0285(14) 0.0018(11) 0.0005(11) 0.0115(11)
C55 0.0563(18) 0.0148(12) 0.0332(15) 0.0020(11) 0.0109(13) 0.0064(12)
C17 0.0230(13) 0.0290(13) 0.0192(12) -0.0021(10) -0.0011(10) -0.0071(10)
C62 0.0403(15) 0.0208(12) 0.0281(14) 0.0009(10) -0.0081(12) 0.0015(11)
C58 0.0416(15) 0.0195(12) 0.0168(12) 0.0011(10) -0.0001(11) 0.0006(11)
C12 0.0292(14) 0.0243(12) 0.0300(14) -0.0098(11) 0.0012(11) 0.0071(10)
C53 0.0413(15) 0.0105(11) 0.0196(12) -0.0002(9) 0.0033(11) -0.0017(10)
C7 0.0238(13) 0.0329(13) 0.0289(14) 0.0127(11) 0.0030(11) 0.0045(11)
C15 0.0396(16) 0.0306(14) 0.0231(13) -0.0058(11) 0.0012(11) 0.0065(12)
C18 0.0243(14) 0.0320(14) 0.0399(16) -0.0059(12) -0.0007(12) -0.0045(11)
C56 0.0538(18) 0.0170(12) 0.0261(14) -0.0045(10) 0.0056(13) -0.0062(12)
C31 0.0523(17) 0.0257(13) 0.0184(13) 0.0067(10) -0.0040(12) -0.0036(12)
C30 0.0320(13) 0.0175(11) 0.0190(12) 0.0035(10) 0.0007(10) -0.0029(10)
C14 0.0362(16) 0.0413(15) 0.0324(15) -0.0120(12) 0.0116(12) 0.0062(12)
C22 0.0340(14) 0.0265(13) 0.0208(13) 0.0001(10) 0.0044(11) -0.0071(11)
C41 0.0302(13) 0.0257(12) 0.0170(12) 0.0051(10) 0.0044(10) -0.0084(11)
C13 0.0242(13) 0.0366(14) 0.0417(16) -0.0113(12) 0.0058(12) 0.0042(11)
C33 0.0414(15) 0.0184(12) 0.0266(14) 0.0018(10) 0.0123(12) 0.0051(11)
C36 0.0570(18) 0.0262(13) 0.0339(15) 0.0088(11) -0.0049(13) 0.0158(12)
C54 0.0427(15) 0.0151(12) 0.0267(13) 0.0019(10) 0.0073(11) 0.0032(11)
C32 0.0607(18) 0.0209(13) 0.0197(13) 0.0002(10) 0.0080(13) 0.0028(12)
C57 0.0478(16) 0.0225(13) 0.0225(13) 0.0005(10) 0.0004(12) -0.0029(12)
C35 0.0366(15) 0.0338(14) 0.0245(13) 0.0116(11) -0.0023(11) 0.0086(12)
C42 0.0384(15) 0.0260(13) 0.0249(14) 0.0010(11) 0.0121(11) -0.0085(11)
C47 0.0457(16) 0.0261(13) 0.0287(14) -0.0066(11) 0.0174(12) -0.0057(12)
C26 0.0412(16) 0.0268(13) 0.0263(14) -0.0060(11) 0.0054(12) -0.0055(12)
C59 0.0479(17) 0.0157(12) 0.0482(17) 0.0019(11) -0.0032(13) 0.0108(11)
C19 0.0302(15) 0.0415(16) 0.0518(18) -0.0033(14) -0.0078(13) -0.0025(12)
C46 0.0344(14) 0.0246(13) 0.0297(14) 0.0080(11) 0.0014(11) -0.0028(11)
C50 0.0386(15) 0.0282(13) 0.0334(15) 0.0071(11) 0.0028(12) 0.0088(11)
C45 0.0553(19) 0.0395(16) 0.0345(16) 0.0161(13) 0.0005(14) 0.0041(14)
C23 0.0235(14) 0.0410(16) 0.0582(19) -0.0163(14) -0.0078(13) 0.0067(12)
C21 0.0459(17) 0.0343(15) 0.0275(15) -0.0044(12) -0.0036(13) -0.0140(13)
C63 0.066(2) 0.0277(14) 0.0360(16) 0.0054(12) -0.0145(14) 0.0007(13)
C43 0.070(2) 0.0406(16) 0.0229(15) 0.0008(13) 0.0149(14) -0.0071(15)
C51 0.0436(17) 0.0412(16) 0.0460(17) 0.0106(13) 0.0073(14) 0.0106(13)
C20 0.0381(17) 0.0470(17) 0.0429(17) 0.0023(14) -0.0149(13) -0.0110(14)
C52 0.0477(17) 0.0312(15) 0.0526(18) 0.0034(13) -0.0026(14) 0.0049(13)
C25 0.0466(18) 0.0404(17) 0.078(2) -0.0159(16) -0.0052(16) 0.0214(14)
C40 0.0398(18) 0.0522(19) 0.076(2) 0.0267(17) -0.0130(16) -0.0085(14)
C37 0.0431(17) 0.0543(18) 0.0387(16) 0.0160(14) -0.0104(13) 0.0068(14)
C64 0.063(2) 0.0549(19) 0.0525(19) 0.0188(15) 0.0111(16) 0.0316(16)
C44 0.080(2) 0.0511(19) 0.0262(16) 0.0172(14) 0.0003(15) 0.0018(17)
C61 0.078(2) 0.0265(15) 0.065(2) 0.0121(14) -0.0182(18) 0.0085(15)
C27 0.078(2) 0.0408(16) 0.0342(16) 0.0049(13) 0.0074(15) 0.0129(15)
C28 0.067(2) 0.0403(16) 0.0326(16) -0.0112(13) 0.0157(14) 0.0006(15)
C49 0.066(2) 0.0371(16) 0.0486(18) -0.0139(14) 0.0093(16) -0.0030(15)
C48 0.0471(18) 0.0425(17) 0.069(2) -0.0102(15) 0.0297(16) -0.0046(14)
C60 0.053(2) 0.0358(16) 0.086(2) -0.0004(16) 0.0057(18) 0.0192(15)
C24 0.112(3) 0.087(3) 0.062(2) -0.020(2) 0.030(2) -0.001(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 Cl1 2.2620(6) . ?
Co1 Cl2 2.2559(7) . ?
Co1 C3 2.062(2) . ?
Co1 C1 2.061(2) . ?
N6 N5 1.331(2) . ?
N6 C4 1.369(3) . ?
N6 C53 1.457(3) . ?
N5 N4 1.342(2) . ?
N4 C3 1.374(3) . ?
N4 C29 1.459(2) . ?
N3 N2 1.331(2) . ?
N3 C2 1.377(3) . ?
N3 C41 1.452(3) . ?
N1 N2 1.334(2) . ?
N1 C1 1.380(3) . ?
N1 C17 1.464(3) . ?
C3 C4 1.399(3) . ?
C5 C2 1.475(3) . ?
C5 C10 1.397(3) . ?
C5 C6 1.401(3) . ?
C2 C1 1.390(3) . ?
C4 C11 1.476(3) . ?
C29 C34 1.387(3) . ?
C29 C30 1.403(3) . ?
C11 C16 1.394(3) . ?
C11 C12 1.392(3) . ?
C10 H10 0.9500 . ?
C10 C9 1.388(3) . ?
C34 C38 1.517(3) . ?
C34 C33 1.399(3) . ?
C38 H38 1.0000 . ?
C38 C39 1.525(3) . ?
C38 C40 1.517(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.386(3) . ?
C16 H16 0.9500 . ?
C16 C15 1.386(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.380(3) . ?
C8 C7 1.381(3) . ?
C9 H9 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C55 H55 0.9500 . ?
C55 C56 1.372(4) . ?
C55 C54 1.404(3) . ?
C17 C18 1.387(3) . ?
C17 C22 1.399(3) . ?
C62 H62 1.0000 . ?
C62 C58 1.516(3) . ?
C62 C63 1.520(3) . ?
C62 C64 1.526(4) . ?
C58 C53 1.397(3) . ?
C58 C57 1.397(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.387(3) . ?
C53 C54 1.395(3) . ?
C7 H7 0.9500 . ?
C15 H15 0.9500 . ?
C15 C14 1.383(3) . ?
C18 C19 1.394(3) . ?
C18 C23 1.522(3) . ?
C56 H56 0.9500 . ?
C56 C57 1.379(3) . ?
C31 H31 0.9500 . ?
C31 C30 1.391(3) . ?
C31 C32 1.383(3) . ?
C30 C35 1.515(3) . ?
C14 H14 0.9500 . ?
C14 C13 1.384(3) . ?
C22 C26 1.518(3) . ?
C22 C21 1.396(3) . ?
C41 C42 1.398(3) . ?
C41 C46 1.395(3) . ?
C13 H13 0.9500 . ?
C33 H33 0.9500 . ?
C33 C32 1.379(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C36 C35 1.533(3) . ?
C54 C59 1.516(3) . ?
C32 H32 0.9500 . ?
C57 H57 0.9500 . ?
C35 H35 1.0000 . ?
C35 C37 1.535(3) . ?
C42 C47 1.516(4) . ?
C42 C43 1.399(4) . ?
C47 H47 1.0000 . ?
C47 C49 1.531(3) . ?
C47 C48 1.541(3) . ?
C26 H26 1.0000 . ?
C26 C27 1.526(3) . ?
C26 C28 1.527(3) . ?
C59 H59 1.0000 . ?
C59 C61 1.534(4) . ?
C59 C60 1.536(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.379(3) . ?
C46 C50 1.518(3) . ?
C46 C45 1.395(3) . ?
C50 H50 1.0000 . ?
C50 C51 1.529(3) . ?
C50 C52 1.533(3) . ?
C45 H45 0.9500 . ?
C45 C44 1.379(4) . ?
C23 H23 1.0000 . ?
C23 C25 1.520(4) . ?
C23 C24 1.521(4) . ?
C21 H21 0.9500 . ?
C21 C20 1.377(4) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C43 H43 0.9500 . ?
C43 C44 1.370(4) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C20 H20 0.9500 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C44 H44 0.9500 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Co1 Cl1 117.25(2) . . ?
C3 Co1 Cl1 109.09(6) . . ?
C3 Co1 Cl2 102.81(6) . . ?
C1 Co1 Cl1 101.35(6) . . ?
C1 Co1 Cl2 110.14(6) . . ?
C1 Co1 C3 116.86(8) . . ?
N5 N6 C4 112.45(16) . . ?
N5 N6 C53 118.58(17) . . ?
C4 N6 C53 128.90(17) . . ?
N6 N5 N4 102.43(15) . . ?
N5 N4 C3 116.17(16) . . ?
N5 N4 C29 116.11(16) . . ?
C3 N4 C29 127.70(16) . . ?
N2 N3 C2 111.88(17) . . ?
N2 N3 C41 118.82(17) . . ?
C2 N3 C41 129.15(18) . . ?
N2 N1 C1 115.96(18) . . ?
N2 N1 C17 115.47(17) . . ?
C1 N1 C17 128.57(18) . . ?
N3 N2 N1 102.92(16) . . ?
N4 C3 Co1 127.01(14) . . ?
N4 C3 C4 101.22(17) . . ?
C4 C3 Co1 131.64(15) . . ?
C10 C5 C2 121.84(19) . . ?
C10 C5 C6 119.1(2) . . ?
C6 C5 C2 119.10(19) . . ?
N3 C2 C5 122.00(19) . . ?
N3 C2 C1 107.85(18) . . ?
C1 C2 C5 130.06(19) . . ?
N1 C1 Co1 126.51(15) . . ?
N1 C1 C2 101.38(18) . . ?
C2 C1 Co1 131.62(15) . . ?
N6 C4 C3 107.73(18) . . ?
N6 C4 C11 123.20(18) . . ?
C3 C4 C11 129.05(19) . . ?
C34 C29 N4 117.76(19) . . ?
C34 C29 C30 124.6(2) . . ?
C30 C29 N4 117.68(19) . . ?
C16 C11 C4 122.2(2) . . ?
C12 C11 C4 118.6(2) . . ?
C12 C11 C16 119.2(2) . . ?
C5 C10 H10 119.9 . . ?
C9 C10 C5 120.2(2) . . ?
C9 C10 H10 119.9 . . ?
C29 C34 C38 123.22(19) . . ?
C29 C34 C33 116.7(2) . . ?
C33 C34 C38 120.1(2) . . ?
C34 C38 H38 107.9 . . ?
C34 C38 C39 112.32(18) . . ?
C39 C38 H38 107.9 . . ?
C40 C38 C34 110.0(2) . . ?
C40 C38 H38 107.9 . . ?
C40 C38 C39 110.6(2) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 C5 119.9(2) . . ?
C7 C6 H6 120.1 . . ?
C11 C16 H16 119.8 . . ?
C15 C16 C11 120.4(2) . . ?
C15 C16 H16 119.8 . . ?
C9 C8 H8 120.0 . . ?
C9 C8 C7 120.0(2) . . ?
C7 C8 H8 120.0 . . ?
C10 C9 H9 119.9 . . ?
C8 C9 C10 120.2(2) . . ?
C8 C9 H9 119.9 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C56 C55 H55 119.5 . . ?
C56 C55 C54 121.0(2) . . ?
C54 C55 H55 119.5 . . ?
C18 C17 N1 118.41(19) . . ?
C18 C17 C22 124.0(2) . . ?
C22 C17 N1 117.5(2) . . ?
C58 C62 H62 108.1 . . ?
C58 C62 C63 112.5(2) . . ?
C58 C62 C64 109.4(2) . . ?
C63 C62 H62 108.1 . . ?
C63 C62 C64 110.5(2) . . ?
C64 C62 H62 108.1 . . ?
C53 C58 C62 123.81(19) . . ?
C57 C58 C62 120.1(2) . . ?
C57 C58 C53 116.0(2) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 120.0(2) . . ?
C13 C12 H12 120.0 . . ?
C58 C53 N6 118.20(19) . . ?
C54 C53 N6 117.5(2) . . ?
C54 C53 C58 124.3(2) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.6(2) . . ?
C8 C7 H7 119.7 . . ?
C16 C15 H15 120.0 . . ?
C14 C15 C16 120.1(2) . . ?
C14 C15 H15 120.0 . . ?
C17 C18 C19 117.0(2) . . ?
C17 C18 C23 123.6(2) . . ?
C19 C18 C23 119.5(2) . . ?
C55 C56 H56 119.6 . . ?
C55 C56 C57 120.7(2) . . ?
C57 C56 H56 119.6 . . ?
C30 C31 H31 119.2 . . ?
C32 C31 H31 119.2 . . ?
C32 C31 C30 121.6(2) . . ?
C29 C30 C35 121.79(19) . . ?
C31 C30 C29 115.8(2) . . ?
C31 C30 C35 122.3(2) . . ?
C15 C14 H14 120.1 . . ?
C15 C14 C13 119.8(2) . . ?
C13 C14 H14 120.1 . . ?
C17 C22 C26 122.8(2) . . ?
C21 C22 C17 116.1(2) . . ?
C21 C22 C26 121.0(2) . . ?
C42 C41 N3 118.1(2) . . ?
C46 C41 N3 117.4(2) . . ?
C46 C41 C42 124.5(2) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.5(2) . . ?
C14 C13 H13 119.8 . . ?
C34 C33 H33 119.7 . . ?
C32 C33 C34 120.7(2) . . ?
C32 C33 H33 119.7 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
C55 C54 C59 119.4(2) . . ?
C53 C54 C55 116.5(2) . . ?
C53 C54 C59 124.1(2) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.6(2) . . ?
C33 C32 H32 119.7 . . ?
C58 C57 H57 119.2 . . ?
C56 C57 C58 121.5(2) . . ?
C56 C57 H57 119.2 . . ?
C30 C35 C36 110.9(2) . . ?
C30 C35 H35 107.6 . . ?
C30 C35 C37 113.4(2) . . ?
C36 C35 H35 107.6 . . ?
C36 C35 C37 109.4(2) . . ?
C37 C35 H35 107.6 . . ?
C41 C42 C47 122.1(2) . . ?
C41 C42 C43 116.1(2) . . ?
C43 C42 C47 121.8(2) . . ?
C42 C47 H47 107.9 . . ?
C42 C47 C49 112.9(2) . . ?
C42 C47 C48 110.2(2) . . ?
C49 C47 H47 107.9 . . ?
C49 C47 C48 110.0(2) . . ?
C48 C47 H47 107.9 . . ?
C22 C26 H26 108.2 . . ?
C22 C26 C27 109.7(2) . . ?
C22 C26 C28 113.2(2) . . ?
C27 C26 H26 108.2 . . ?
C27 C26 C28 109.1(2) . . ?
C28 C26 H26 108.2 . . ?
C54 C59 H59 107.7 . . ?
C54 C59 C61 111.0(2) . . ?
C54 C59 C60 111.4(2) . . ?
C61 C59 H59 107.7 . . ?
C61 C59 C60 111.1(2) . . ?
C60 C59 H59 107.7 . . ?
C18 C19 H19 119.5 . . ?
C20 C19 C18 121.1(3) . . ?
C20 C19 H19 119.5 . . ?
C41 C46 C50 123.5(2) . . ?
C45 C46 C41 116.2(2) . . ?
C45 C46 C50 120.3(2) . . ?
C46 C50 H50 107.9 . . ?
C46 C50 C51 112.1(2) . . ?
C46 C50 C52 110.3(2) . . ?
C51 C50 H50 107.9 . . ?
C51 C50 C52 110.7(2) . . ?
C52 C50 H50 107.9 . . ?
C46 C45 H45 119.5 . . ?
C44 C45 C46 121.1(3) . . ?
C44 C45 H45 119.5 . . ?
C18 C23 H23 107.8 . . ?
C25 C23 C18 112.6(2) . . ?
C25 C23 H23 107.8 . . ?
C25 C23 C24 109.5(3) . . ?
C24 C23 C18 111.1(2) . . ?
C24 C23 H23 107.8 . . ?
C22 C21 H21 119.2 . . ?
C20 C21 C22 121.6(2) . . ?
C20 C21 H21 119.2 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C42 C43 H43 119.5 . . ?
C44 C43 C42 121.0(2) . . ?
C44 C43 H43 119.5 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.2(2) . . ?
C21 C20 H20 119.9 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C45 C44 H44 119.5 . . ?
C43 C44 C45 121.1(3) . . ?
C43 C44 H44 119.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.970 579.8 107.3 ?
_shelx_res_file
;
TITL cocl2mic2_a.res in P-1
cocl2mic2.res
created by SHELXL-2016/6 at 14:33:58 on 18-Oct-2019
REM Old TITL CoCl2MIC2 in P-1
REM SHELXT solution in P-1
REM R1 0.173, Rweak 0.012, Alpha 0.079, Orientation as input
REM Formula found by SHELXT: C65 N7 Cl2 Co
CELL 0.71073 13.6433 15.2982 15.8757 97.413 91.715 97.494
ZERR 2 0.001 0.0011 0.0012 0.002 0.003 0.002
LATT 1
SFAC C H Cl Co N
UNIT 128 156 4 2 12
L.S. 4
PLAN 20
TEMP -173.15
BOND $H
list 4
ABIN
fmap 2
acta
OMIT 0 1 0
REM
REM
REM
WGHT 0.045100 0.300700
FVAR 0.31872
CO1 4 0.251880 0.667390 0.647642 11.00000 0.02016 0.01604 =
0.01750 -0.00050 0.00123 0.00399
CL1 3 0.312849 0.546603 0.583219 11.00000 0.03056 0.02035 =
0.03006 -0.00279 0.00717 0.00684
CL2 3 0.123212 0.712581 0.580544 11.00000 0.02773 0.03086 =
0.03470 0.00211 -0.00757 0.00729
N6 5 0.456451 0.906770 0.688100 11.00000 0.02929 0.01207 =
0.01889 0.00169 0.00159 0.00364
N5 5 0.485436 0.874179 0.612506 11.00000 0.02811 0.01447 =
0.01888 0.00134 0.00127 0.00223
N4 5 0.425580 0.796614 0.594904 11.00000 0.02218 0.01248 =
0.01729 0.00089 -0.00079 0.00390
N3 5 0.201003 0.578187 0.888343 11.00000 0.02238 0.01947 =
0.01851 -0.00066 0.00423 0.00026
N1 5 0.119805 0.576568 0.774692 11.00000 0.02283 0.01975 =
0.01843 -0.00343 0.00456 -0.00038
N2 5 0.112730 0.547555 0.850279 11.00000 0.02489 0.02303 =
0.02039 -0.00330 0.00458 -0.00168
C3 1 0.359440 0.776502 0.655396 11.00000 0.01979 0.01775 =
0.01601 0.00429 -0.00132 0.01002
C5 1 0.364130 0.663407 0.864174 11.00000 0.02294 0.01629 =
0.01938 0.00526 0.00026 0.00031
C2 1 0.261257 0.625673 0.837289 11.00000 0.02161 0.01317 =
0.01706 0.00018 0.00565 0.00208
C1 1 0.208969 0.625079 0.760696 11.00000 0.01807 0.01438 =
0.02078 -0.00508 0.00407 0.00119
C4 1 0.381740 0.851196 0.716950 11.00000 0.02310 0.01551 =
0.01924 0.00439 0.00100 0.00610
C29 1 0.440104 0.742685 0.514674 11.00000 0.02884 0.01314 =
0.01586 0.00074 0.00587 -0.00105
C11 1 0.335166 0.872545 0.798471 11.00000 0.02681 0.01441 =
0.02295 -0.00015 0.00301 0.00751
C10 1 0.389577 0.706872 0.946311 11.00000 0.02761 0.02184 =
0.02112 0.00283 0.00335 0.00038
AFIX 43
H10 2 0.339663 0.713812 0.986158 11.00000 -1.20000
AFIX 0
C34 1 0.514575 0.688904 0.513155 11.00000 0.02904 0.01414 =
0.02326 0.00319 0.00570 0.00125
C38 1 0.582610 0.685680 0.589755 11.00000 0.02581 0.02001 =
0.02560 -0.00084 0.00195 0.00702
AFIX 13
H38 2 0.556501 0.719839 0.640244 11.00000 -1.20000
AFIX 0
C6 1 0.438486 0.655207 0.805844 11.00000 0.02641 0.02215 =
0.02269 0.00666 -0.00073 0.00435
AFIX 43
H6 2 0.422290 0.626217 0.749629 11.00000 -1.20000
AFIX 0
C16 1 0.390431 0.909573 0.872739 11.00000 0.02593 0.02341 =
0.02516 0.00093 0.00097 0.00576
AFIX 43
H16 2 0.460394 0.922201 0.871641 11.00000 -1.20000
AFIX 0
C8 1 0.560264 0.730828 0.912126 11.00000 0.02267 0.03198 =
0.03093 0.01381 -0.00644 -0.00303
AFIX 43
H8 2 0.627307 0.753028 0.928659 11.00000 -1.20000
AFIX 0
C9 1 0.487484 0.739942 0.969903 11.00000 0.03294 0.02692 =
0.02305 0.00412 -0.00575 -0.00470
AFIX 43
H9 2 0.504465 0.768946 1.025999 11.00000 -1.20000
AFIX 0
C39 1 0.585970 0.590949 0.608907 11.00000 0.03498 0.02403 =
0.02855 0.00185 0.00046 0.01152
AFIX 137
H39A 2 0.518850 0.563080 0.617614 11.00000 -1.50000
H39B 2 0.627846 0.592324 0.660431 11.00000 -1.50000
H39C 2 0.613373 0.556560 0.560986 11.00000 -1.50000
AFIX 0
C55 1 0.491018 1.148852 0.764179 11.00000 0.05632 0.01479 =
0.03319 0.00198 0.01093 0.00640
AFIX 43
H55 2 0.456313 1.198791 0.764070 11.00000 -1.20000
AFIX 0
C17 1 0.031729 0.552229 0.717337 11.00000 0.02301 0.02899 =
0.01921 -0.00208 -0.00108 -0.00712
C62 1 0.658695 0.927511 0.762565 11.00000 0.04028 0.02083 =
0.02807 0.00087 -0.00809 0.00149
AFIX 13
H62 2 0.614955 0.870940 0.740841 11.00000 -1.20000
AFIX 0
C58 1 0.597070 1.003290 0.764746 11.00000 0.04156 0.01951 =
0.01675 0.00114 -0.00005 0.00063
C12 1 0.232819 0.853257 0.801237 11.00000 0.02921 0.02431 =
0.02997 -0.00977 0.00124 0.00709
AFIX 43
H12 2 0.194376 0.827526 0.751160 11.00000 -1.20000
AFIX 0
C53 1 0.502017 0.994841 0.726716 11.00000 0.04133 0.01046 =
0.01956 -0.00015 0.00327 -0.00172
C7 1 0.535705 0.689454 0.830282 11.00000 0.02381 0.03293 =
0.02892 0.01265 0.00301 0.00446
AFIX 43
H7 2 0.585889 0.684434 0.790409 11.00000 -1.20000
AFIX 0
C15 1 0.343983 0.928095 0.948195 11.00000 0.03960 0.03059 =
0.02312 -0.00577 0.00117 0.00647
AFIX 43
H15 2 0.382073 0.953953 0.998420 11.00000 -1.20000
AFIX 0
C18 1 -0.040776 0.608114 0.722212 11.00000 0.02426 0.03197 =
0.03989 -0.00593 -0.00065 -0.00448
C56 1 0.583239 1.159392 0.804093 11.00000 0.05383 0.01696 =
0.02609 -0.00448 0.00562 -0.00617
AFIX 43
H56 2 0.611223 1.216313 0.831859 11.00000 -1.20000
AFIX 0
C31 1 0.392188 0.694468 0.369885 11.00000 0.05234 0.02572 =
0.01841 0.00667 -0.00403 -0.00357
AFIX 43
H31 2 0.350763 0.694933 0.320813 11.00000 -1.20000
AFIX 0
C30 1 0.377085 0.748198 0.444638 11.00000 0.03199 0.01752 =
0.01896 0.00348 0.00073 -0.00295
C14 1 0.242282 0.908980 0.950451 11.00000 0.03624 0.04132 =
0.03240 -0.01195 0.01158 0.00623
AFIX 43
H14 2 0.210451 0.921461 1.002200 11.00000 -1.20000
AFIX 0
C22 1 0.024769 0.472158 0.662481 11.00000 0.03400 0.02646 =
0.02084 0.00011 0.00443 -0.00706
C41 1 0.223735 0.553801 0.971462 11.00000 0.03021 0.02568 =
0.01703 0.00505 0.00438 -0.00836
C13 1 0.186987 0.871596 0.877062 11.00000 0.02420 0.03658 =
0.04169 -0.01126 0.00582 0.00421
AFIX 43
H13 2 0.117123 0.858409 0.878666 11.00000 -1.20000
AFIX 0
C33 1 0.526837 0.637580 0.435582 11.00000 0.04139 0.01836 =
0.02658 0.00177 0.01230 0.00513
AFIX 43
H33 2 0.577570 0.600413 0.431310 11.00000 -1.20000
AFIX 0
C36 1 0.348791 0.906747 0.442557 11.00000 0.05704 0.02621 =
0.03388 0.00882 -0.00486 0.01578
AFIX 137
H36A 2 0.403601 0.923961 0.485261 11.00000 -1.50000
H36B 2 0.299571 0.947798 0.452299 11.00000 -1.50000
H36C 2 0.374030 0.909153 0.385637 11.00000 -1.50000
AFIX 0
C54 1 0.447226 1.065340 0.723506 11.00000 0.04274 0.01515 =
0.02673 0.00187 0.00730 0.00318
C32 1 0.466045 0.640385 0.365262 11.00000 0.06071 0.02090 =
0.01967 0.00018 0.00796 0.00278
AFIX 43
H32 2 0.475006 0.604819 0.313157 11.00000 -1.20000
AFIX 0
C57 1 0.635715 1.088229 0.804322 11.00000 0.04779 0.02246 =
0.02248 0.00052 0.00038 -0.00288
AFIX 43
H57 2 0.699610 1.097169 0.832027 11.00000 -1.20000
AFIX 0
C35 1 0.300573 0.811860 0.449552 11.00000 0.03658 0.03378 =
0.02453 0.01164 -0.00228 0.00858
AFIX 13
H35 2 0.271512 0.812381 0.506670 11.00000 -1.20000
AFIX 0
C42 1 0.185969 0.599708 1.042472 11.00000 0.03843 0.02602 =
0.02492 0.00100 0.01205 -0.00853
C47 1 0.117625 0.669057 1.034432 11.00000 0.04575 0.02609 =
0.02872 -0.00661 0.01741 -0.00574
AFIX 13
H47 2 0.125901 0.689271 0.977315 11.00000 -1.20000
AFIX 0
C26 1 0.101924 0.409128 0.662925 11.00000 0.04120 0.02682 =
0.02630 -0.00598 0.00535 -0.00546
AFIX 13
H26 2 0.166264 0.444444 0.685693 11.00000 -1.20000
AFIX 0
C59 1 0.347184 1.057186 0.676799 11.00000 0.04790 0.01571 =
0.04820 0.00191 -0.00321 0.01075
AFIX 13
H59 2 0.328409 0.993425 0.652215 11.00000 -1.20000
AFIX 0
C19 1 -0.125133 0.581546 0.668689 11.00000 0.03016 0.04148 =
0.05184 -0.00332 -0.00784 -0.00253
AFIX 43
H19 2 -0.176961 0.617538 0.670858 11.00000 -1.20000
AFIX 0
C46 1 0.283008 0.486486 0.974873 11.00000 0.03435 0.02463 =
0.02972 0.00803 0.00135 -0.00285
C50 1 0.317954 0.433619 0.896541 11.00000 0.03861 0.02822 =
0.03338 0.00710 0.00276 0.00876
AFIX 13
H50 2 0.292957 0.457449 0.845423 11.00000 -1.20000
AFIX 0
C45 1 0.308305 0.467954 1.055848 11.00000 0.05530 0.03955 =
0.03447 0.01611 0.00054 0.00410
AFIX 43
H45 2 0.349981 0.423758 1.061719 11.00000 -1.20000
AFIX 0
C23 1 -0.033128 0.694399 0.783135 11.00000 0.02345 0.04097 =
0.05818 -0.01632 -0.00782 0.00673
AFIX 13
H23 2 0.034380 0.705061 0.811910 11.00000 -1.20000
AFIX 0
C21 1 -0.060468 0.450632 0.609020 11.00000 0.04591 0.03426 =
0.02748 -0.00442 -0.00361 -0.01396
AFIX 43
H21 2 -0.067476 0.397983 0.569195 11.00000 -1.20000
AFIX 0
C63 1 0.701637 0.918349 0.849951 11.00000 0.06574 0.02767 =
0.03598 0.00537 -0.01449 0.00066
AFIX 137
H63A 2 0.748571 0.971414 0.870710 11.00000 -1.50000
H63B 2 0.735944 0.865641 0.846058 11.00000 -1.50000
H63C 2 0.648083 0.912084 0.889424 11.00000 -1.50000
AFIX 0
C43 1 0.212855 0.576355 1.121498 11.00000 0.06974 0.04063 =
0.02287 0.00081 0.01486 -0.00706
AFIX 43
H43 2 0.188482 0.605037 1.171721 11.00000 -1.20000
AFIX 0
C51 1 0.430816 0.443212 0.895314 11.00000 0.04363 0.04118 =
0.04604 0.01059 0.00731 0.01062
AFIX 137
H51A 2 0.457407 0.506183 0.897474 11.00000 -1.50000
H51B 2 0.450222 0.409768 0.843004 11.00000 -1.50000
H51C 2 0.457176 0.419836 0.944678 11.00000 -1.50000
AFIX 0
C20 1 -0.134584 0.503859 0.612632 11.00000 0.03810 0.04703 =
0.04294 0.00228 -0.01494 -0.01104
AFIX 43
H20 2 -0.192451 0.487008 0.576375 11.00000 -1.20000
AFIX 0
C52 1 0.273860 0.335451 0.890454 11.00000 0.04768 0.03122 =
0.05263 0.00337 -0.00261 0.00489
AFIX 137
H52A 2 0.298082 0.310238 0.939531 11.00000 -1.50000
H52B 2 0.293805 0.302726 0.837970 11.00000 -1.50000
H52C 2 0.201505 0.330632 0.889971 11.00000 -1.50000
AFIX 0
C25 1 -0.045783 0.774243 0.737898 11.00000 0.04661 0.04042 =
0.07772 -0.01589 -0.00525 0.02145
AFIX 137
H25A 2 0.002994 0.779014 0.694073 11.00000 -1.50000
H25B 2 -0.035858 0.828466 0.779143 11.00000 -1.50000
H25C 2 -0.112642 0.766717 0.711319 11.00000 -1.50000
AFIX 0
C40 1 0.685752 0.730712 0.576540 11.00000 0.03978 0.05222 =
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AFIX 137
H40A 2 0.714897 0.695948 0.529899 11.00000 -1.50000
H40B 2 0.727098 0.734583 0.628790 11.00000 -1.50000
H40C 2 0.681896 0.790697 0.562393 11.00000 -1.50000
AFIX 0
C37 1 0.215366 0.784697 0.382105 11.00000 0.04311 0.05427 =
0.03865 0.01605 -0.01044 0.00679
AFIX 137
H37A 2 0.240188 0.791662 0.325729 11.00000 -1.50000
H37B 2 0.163523 0.822658 0.394086 11.00000 -1.50000
H37C 2 0.187976 0.722425 0.383429 11.00000 -1.50000
AFIX 0
C64 1 0.741129 0.940946 0.700732 11.00000 0.06265 0.05495 =
0.05245 0.01878 0.01108 0.03164
AFIX 137
H64A 2 0.712036 0.941208 0.643587 11.00000 -1.50000
H64B 2 0.781556 0.892409 0.699857 11.00000 -1.50000
H64C 2 0.782733 0.997848 0.719041 11.00000 -1.50000
AFIX 0
C44 1 0.273779 0.512771 1.127542 11.00000 0.08024 0.05112 =
0.02624 0.01716 0.00034 0.00183
AFIX 43
H44 2 0.292563 0.499320 1.182022 11.00000 -1.20000
AFIX 0
C61 1 0.352460 1.112894 0.602910 11.00000 0.07781 0.02646 =
0.06481 0.01205 -0.01824 0.00853
AFIX 137
H61A 2 0.366129 1.176195 0.625494 11.00000 -1.50000
H61B 2 0.289160 1.101385 0.569935 11.00000 -1.50000
H61C 2 0.405462 1.096680 0.566112 11.00000 -1.50000
AFIX 0
C27 1 0.072095 0.339923 0.721858 11.00000 0.07793 0.04080 =
0.03421 0.00490 0.00741 0.01290
AFIX 137
H27A 2 0.064255 0.370040 0.779109 11.00000 -1.50000
H27B 2 0.123538 0.301034 0.723989 11.00000 -1.50000
H27C 2 0.009330 0.304246 0.700332 11.00000 -1.50000
AFIX 0
C28 1 0.117569 0.361578 0.574738 11.00000 0.06715 0.04026 =
0.03256 -0.01121 0.01565 0.00057
AFIX 137
H28A 2 0.057308 0.321573 0.553866 11.00000 -1.50000
H28B 2 0.172855 0.327004 0.578070 11.00000 -1.50000
H28C 2 0.132586 0.405630 0.535666 11.00000 -1.50000
AFIX 0
C49 1 0.141316 0.750827 1.101824 11.00000 0.06645 0.03708 =
0.04861 -0.01393 0.00930 -0.00302
AFIX 137
H49A 2 0.127345 0.733796 1.158123 11.00000 -1.50000
H49B 2 0.100369 0.796229 1.089755 11.00000 -1.50000
H49C 2 0.211404 0.774813 1.100745 11.00000 -1.50000
AFIX 0
C48 1 0.009021 0.627611 1.038671 11.00000 0.04709 0.04251 =
0.06880 -0.01023 0.02966 -0.00457
AFIX 137
H48A 2 -0.007644 0.579589 0.991310 11.00000 -1.50000
H48B 2 -0.034380 0.673317 1.034757 11.00000 -1.50000
H48C 2 0.000010 0.603566 1.092641 11.00000 -1.50000
AFIX 0
C60 1 0.266947 1.082714 0.737595 11.00000 0.05349 0.03575 =
0.08600 -0.00036 0.00569 0.01918
AFIX 137
H60A 2 0.266112 1.047241 0.784812 11.00000 -1.50000
H60B 2 0.202236 1.071141 0.706833 11.00000 -1.50000
H60C 2 0.281305 1.146044 0.759922 11.00000 -1.50000
AFIX 0
C24 1 -0.108436 0.687326 0.851481 11.00000 0.11230 0.08741 =
0.06233 -0.02045 0.02964 -0.00118
AFIX 137
H24A 2 -0.175427 0.679483 0.825122 11.00000 -1.50000
H24B 2 -0.098474 0.741792 0.892409 11.00000 -1.50000
H24C 2 -0.099938 0.636146 0.880955 11.00000 -1.50000
AFIX 0
HKLF 4
REM cocl2mic2_a.res in P-1
REM R1 = 0.0448 for 8931 Fo > 4sig(Fo) and 0.0811 for all 13291 data
REM 674 parameters refined using 0 restraints
END
WGHT 0.0449 0.3136
REM Highest difference peak 0.786, deepest hole -0.269, 1-sigma level 0.055
Q1 1 0.4923 0.5895 0.2755 11.00000 0.05 0.79
Q2 1 0.0346 0.6228 1.0917 11.00000 0.05 0.29
Q3 1 0.4422 0.7151 0.9542 11.00000 0.05 0.26
Q4 1 0.3618 0.8587 0.7605 11.00000 0.05 0.26
Q5 1 -0.1277 0.6874 0.8342 11.00000 0.05 0.26
Q6 1 0.4973 0.9585 0.7019 11.00000 0.05 0.25
Q7 1 0.3881 0.6593 0.9082 11.00000 0.05 0.24
Q8 1 0.2825 0.8808 0.7918 11.00000 0.05 0.24
Q9 1 0.0867 0.3777 0.6932 11.00000 0.05 0.23
Q10 1 0.5556 0.6817 0.4650 11.00000 0.05 0.23
Q11 1 0.7564 0.9259 0.9043 11.00000 0.05 0.22
Q12 1 0.5556 0.6802 0.5472 11.00000 0.05 0.22
Q13 1 -0.1436 0.6351 0.6064 11.00000 0.05 0.22
Q14 1 0.3158 0.6343 0.8538 11.00000 0.05 0.22
Q15 1 0.2769 0.4610 1.0067 11.00000 0.05 0.22
Q16 1 0.3337 0.7226 0.6520 11.00000 0.05 0.22
Q17 1 0.4096 0.7126 0.3490 11.00000 0.05 0.22
Q18 1 0.1078 0.7989 0.6053 11.00000 0.05 0.21
Q19 1 -0.0293 0.4383 0.5677 11.00000 0.05 0.21
Q20 1 0.4274 0.7558 0.4732 11.00000 0.05 0.21
;
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15 -6 7 -1.2909 0.0263
15 -6 8 -2.5931 -0.0702
15 -5 0 -3.1548 -0.0301
15 -5 1 -0.6312 0.0094
15 -5 2 0.4235 0.0324
15 -5 3 -0.7211 -0.0253
15 -5 4 0.3742 0.0297
15 -5 5 0.0923 0.0009
15 -5 6 0.2987 0.0923
15 -5 7 0.2374 0.0132
15 -5 8 -1.9702 0.0688
15 -4 0 -2.2723 0.0274
15 -4 1 -2.7108 0.0178
15 -4 2 0.8444 0.0025
15 -4 3 -0.0774 0.0171
15 -4 4 -0.4401 0.0059
15 -4 5 -0.0815 -0.0125
15 -4 6 -0.4790 0.0737
15 -4 7 1.6294 -0.0147
15 -4 8 -1.3093 0.0364
15 -3 0 -0.4361 0.0473
15 -3 1 -1.8693 0.0260
15 -3 2 0.1566 -0.0002
15 -3 3 -0.6182 -0.0147
15 -3 4 0.0784 -0.0050
15 -3 5 -0.2162 -0.0005
15 -3 6 -0.4515 -0.0187
15 -3 7 0.5651 0.0391
15 -3 8 -0.3482 -0.0352
15 -2 0 0.4290 0.0257
15 -2 1 0.4704 -0.0201
15 -2 2 -0.2482 -0.0057
15 -2 3 -0.6806 -0.0091
15 -2 4 0.3988 -0.0358
15 -2 5 -0.7834 0.0198
15 -2 6 0.3579 -0.0237
15 -2 7 0.5042 -0.0083
15 -2 8 -0.6667 0.0238
15 -1 0 0.2110 -0.0293
15 -1 1 2.1146 -0.0006
15 -1 2 -0.4652 -0.0284
15 -1 3 -0.2681 0.0114
15 -1 4 -0.1391 0.0149
15 -1 5 -0.4221 -0.0036
15 -1 6 -0.2223 0.0375
15 -1 7 0.1494 -0.0283
15 -1 8 -0.0449 -0.0190
15 0 0 -0.3028 -0.0382
15 0 1 1.4280 -0.0014
15 0 2 -0.4148 0.0176
15 0 3 0.4966 0.0182
15 0 4 -0.3267 0.0422
15 0 5 -0.4382 0.0310
15 0 6 -0.9732 0.0200
15 0 7 -0.1548 -0.0034
15 0 8 -0.9333 -0.0630
15 1 0 0.1509 0.0089
15 1 1 -0.0003 0.0011
15 1 2 0.0358 0.0284
15 1 3 0.5222 0.0318
15 1 4 0.6679 -0.0120
15 1 5 0.2042 0.0366
15 1 6 -1.5668 0.0144
15 1 7 -0.4934 0.0098
15 2 0 0.4631 0.0028
15 2 1 0.0185 -0.0093
15 2 2 -0.2182 0.0407
15 2 3 0.5808 0.0219
15 2 4 2.0832 -0.0849
15 2 5 0.4051 0.0179
15 2 6 -0.8158 -0.0125
15 2 7 -0.6743 0.0423
15 3 0 -0.6053 0.0107
15 3 1 1.2272 -0.0364
15 3 2 0.1764 0.0389
15 3 3 -0.0804 0.0397
15 3 4 2.3038 -0.1050
15 3 5 1.0718 -0.0127
15 3 6 -0.2589 0.0243
15 4 0 0.3622 -0.0335
15 4 1 0.7379 -0.0124
15 4 2 0.3173 0.0476
15 4 3 1.4343 -0.0098
15 4 4 1.1277 -0.0177
15 4 5 0.7789 -0.0407
15 5 0 2.1525 -0.0687
15 5 1 1.7348 -0.0110
15 5 2 -0.4372 0.0342
15 5 3 1.6611 -0.0546
15 5 4 1.4105 -0.0181
15 6 0 1.1614 -0.0876
15 6 1 1.5114 0.0762
15 6 2 0.5647 -0.0686
16 -8 0 -1.2580 0.1076
16 -8 1 1.0672 0.0602
16 -8 2 -2.4011 -0.0654
16 -8 3 -1.3123 0.1327
16 -7 0 -1.6250 0.0549
16 -7 1 1.1258 -0.0100
16 -7 2 -2.1414 -0.0182
16 -7 3 -1.4065 0.0681
16 -7 4 2.2017 -0.0573
16 -7 5 -1.3083 0.1192
16 -6 0 -2.2004 -0.0268
16 -6 1 1.1181 -0.0283
16 -6 2 -0.2745 0.0171
16 -6 3 -1.8476 -0.0211
16 -6 4 1.2656 0.0126
16 -6 5 0.0182 0.0488
16 -5 0 -2.0850 0.0122
16 -5 1 -1.1832 -0.0226
16 -5 2 1.5894 0.0198
16 -5 3 -0.1504 -0.0094
16 -5 4 -0.8478 0.0158
16 -5 5 -0.2444 -0.0355
16 -5 6 0.0066 0.1338
16 -4 0 -0.7679 0.0758
16 -4 1 -1.7312 -0.0035
16 -4 2 1.2063 0.0234
16 -4 3 0.6525 -0.0305
16 -4 4 -0.2809 0.0169
16 -4 5 -0.8675 -0.0369
16 -4 6 -1.0928 0.0125
16 -3 0 -0.5978 0.0774
16 -3 1 -0.4250 -0.0588
16 -3 2 0.9314 0.0115
16 -3 3 0.0750 -0.0202
16 -3 4 1.0328 -0.0322
16 -3 5 -0.9248 0.0190
16 -3 6 -0.7133 -0.0368
16 -2 0 -0.9253 -0.0071
16 -2 1 0.9949 -0.0190
16 -2 2 0.5568 -0.0683
16 -2 3 -0.7927 0.0023
16 -2 4 1.4593 0.0070
16 -2 5 -0.2907 0.0031
16 -2 6 -0.1344 0.0428
16 -1 0 -1.2287 -0.0740
16 -1 1 1.0587 0.0309
16 -1 2 0.1420 -0.0370
16 -1 3 -0.8182 -0.0011
16 -1 4 0.6844 0.0536
16 -1 5 -0.4328 0.0210
16 0 0 -0.1602 0.0170
16 0 1 0.4383 0.0420
16 0 2 -0.1592 0.0074
16 0 3 -0.5302 0.0234
16 0 4 0.4728 0.0132
16 0 5 -0.4422 0.0386
16 1 0 1.0210 0.0773
16 1 1 0.5657 0.0394
16 1 2 -0.4447 0.0379
16 1 3 0.2015 0.0198
16 1 4 1.0027 -0.0745
16 2 0 0.3797 0.0762
16 2 1 1.6513 -0.0019
16 2 2 -0.0492 0.0450
16 2 3 -0.3528 0.0471
16 2 4 1.8702 -0.1528
16 3 0 0.0776 -0.0085
16 3 1 0.7674 -0.0084
16 3 2 0.7675 0.0555
16 4 0 1.1126 -0.0698
17 -4 0 -0.3101 0.1282
17 -3 0 -0.8101 0.0876
17 -3 1 -0.1433 -0.0578
17 -2 0 -1.1911 -0.0419
17 -2 1 0.1337 0.0292
17 -1 0 -0.6292 -0.0103
0 0 0 0.0 0.0
;
_shelx_fab_checksum 3255
_olex2_exptl_crystal_mounting_method 'suspended in paratone on nylon loop'
_olex2_submission_original_sample_id JR_224
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical Moisture-sensitive
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_cobr2mic2
_database_code_depnum_ccdc_archive 'CCDC 1959509'
loop_
_audit_author_name
_audit_author_address
'Milan Gembicky'
;University of California, San Diego
United States of America
;
_audit_update_record
;
2019-10-18 deposited with the CCDC. 2020-02-06 downloaded from the CCDC.
;
_audit_creation_date 2019-10-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic
'(1,3-bis(2,6-diisopropylphenyl)-5-phenyl-2,3-dihydro-1H-1,2,3-triazol-4-yl)(1-(2,6-diisopropylphenyl)-3-(2-ethyl-6-isopropylphenyl)-5-phenyl-2,3-dihydro-1H-1,2,3-triazol-4-yl)cobalt(II) bromide'
_chemical_formula_moiety 'C64 H78 Br2 Co N6'
_chemical_formula_sum 'C64 H78 Br2 Co N6'
_chemical_formula_weight 1150.07
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.5223(7)
_cell_length_b 19.7040(11)
_cell_length_c 24.1592(13)
_cell_angle_alpha 90
_cell_angle_beta 91.4890(10)
_cell_angle_gamma 90
_cell_volume 5959.0(6)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 5303
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 20.50
_cell_measurement_theta_min 2.53
_shelx_estimated_absorpt_T_max 0.967
_shelx_estimated_absorpt_T_min 0.753
_exptl_absorpt_coefficient_mu 1.672
_exptl_absorpt_correction_T_max 0.7453
_exptl_absorpt_correction_T_min 0.6562
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0689 before and 0.0550 after correction. The Ratio of minimum to maximum transmission is 0.8805. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'greenish blue'
_exptl_crystal_colour_modifier greenish
_exptl_crystal_colour_primary blue
_exptl_crystal_density_diffrn 1.282
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description trapezoid
_exptl_crystal_F_000 2404
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.02
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1333
_diffrn_reflns_av_unetI/netI 0.1036
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_number 65076
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.705
_diffrn_reflns_theta_min 1.334
_diffrn_ambient_temperature 100.0
_diffrn_detector 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 8.258
_diffrn_detector_type 'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type 'Bruker APEX II Ultra'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe X-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Micro Focus Rotating Anode'
_diffrn_source_type 'Bruker TXS'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6531
_reflns_number_total 11339
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection 'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction 'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.690
_refine_diff_density_min -0.777
_refine_diff_density_rms 0.087
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.004
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 674
_refine_ls_number_reflns 11339
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1206
_refine_ls_R_factor_gt 0.0509
_refine_ls_restrained_S_all 1.004
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+3.0918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0870
_refine_ls_wR_factor_ref 0.1067
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
C23(H23), C26(H26), C35(H35), C38(H38), C47(H47), C50(H50), C59(H59), C62(H62)
2.b Aromatic/amide H refined with riding coordinates:
C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C31(H31), C32(H32), C33(H33),
C43(H43), C44(H44), C45(H45), C55(H55), C56(H56), C57(H57)
2.c Idealised Me refined as rotating group:
C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
H28C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,
H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C),
C52(H52A,H52B,H52C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,
H63C), C64(H64A,H64B,H64C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.44582(4) 0.88968(2) 0.70401(2) 0.04620(16) Uani 1 1 d . . . . .
Br2 Br 0.69385(3) 0.78169(2) 0.64521(2) 0.02972(13) Uani 1 1 d . . . . .
Co1 Co 0.52188(4) 0.77932(3) 0.68820(2) 0.01856(14) Uani 1 1 d . . . . .
N1 N 0.3935(2) 0.74784(15) 0.58230(13) 0.0158(7) Uani 1 1 d . . . . .
N2 N 0.3025(2) 0.72597(15) 0.55827(13) 0.0180(7) Uani 1 1 d . . . . .
N3 N 0.2541(2) 0.69584(14) 0.59976(13) 0.0153(7) Uani 1 1 d . . . . .
N4 N 0.5898(2) 0.76058(15) 0.81095(13) 0.0179(8) Uani 1 1 d . . . . .
N5 N 0.6227(2) 0.71757(16) 0.85086(13) 0.0192(7) Uani 1 1 d . . . . .
N6 N 0.6104(2) 0.65765(16) 0.82670(13) 0.0197(8) Uani 1 1 d . . . . .
C1 C 0.4072(3) 0.73491(18) 0.63782(15) 0.0156(9) Uani 1 1 d . . . . .
C2 C 0.3140(3) 0.69826(17) 0.64848(16) 0.0147(9) Uani 1 1 d . . . . .
C3 C 0.5574(3) 0.73166(19) 0.76157(16) 0.0187(9) Uani 1 1 d . . . . .
C4 C 0.5712(3) 0.66294(19) 0.77327(16) 0.0181(9) Uani 1 1 d . . . . .
C5 C 0.2767(3) 0.66567(19) 0.69936(16) 0.0174(9) Uani 1 1 d . . . . .
C6 C 0.2907(3) 0.6981(2) 0.75017(17) 0.0240(10) Uani 1 1 d . . . . .
H6 H 0.325335 0.740947 0.752233 0.029 Uiso 1 1 calc R . . . .
C7 C 0.2539(3) 0.6677(2) 0.79784(17) 0.0277(11) Uani 1 1 d . . . . .
H7 H 0.263329 0.689947 0.832504 0.033 Uiso 1 1 calc R . . . .
C8 C 0.2037(3) 0.6052(2) 0.79530(17) 0.0284(11) Uani 1 1 d . . . . .
H8 H 0.178662 0.584782 0.828119 0.034 Uiso 1 1 calc R . . . .
C9 C 0.1900(3) 0.5727(2) 0.74523(18) 0.0259(10) Uani 1 1 d . . . . .
H9 H 0.155128 0.529911 0.743365 0.031 Uiso 1 1 calc R . . . .
C10 C 0.2274(3) 0.60256(19) 0.69750(17) 0.0203(9) Uani 1 1 d . . . . .
H10 H 0.219092 0.579557 0.663095 0.024 Uiso 1 1 calc R . . . .
C11 C 0.5433(3) 0.60354(19) 0.73835(17) 0.0206(10) Uani 1 1 d . . . . .
C12 C 0.4767(3) 0.5524(2) 0.75774(18) 0.0270(10) Uani 1 1 d . . . . .
H12 H 0.453524 0.553833 0.794856 0.032 Uiso 1 1 calc R . . . .
C13 C 0.4440(3) 0.4995(2) 0.7234(2) 0.0346(12) Uani 1 1 d . . . . .
H13 H 0.398977 0.464855 0.737083 0.041 Uiso 1 1 calc R . . . .
C14 C 0.4769(4) 0.4972(2) 0.6694(2) 0.0344(12) Uani 1 1 d . . . . .
H14 H 0.454335 0.461232 0.645630 0.041 Uiso 1 1 calc R . . . .
C15 C 0.5430(4) 0.5475(2) 0.65015(18) 0.0348(12) Uani 1 1 d . . . . .
H15 H 0.566019 0.545833 0.613021 0.042 Uiso 1 1 calc R . . . .
C16 C 0.5763(4) 0.6006(2) 0.68417(18) 0.0293(11) Uani 1 1 d . . . . .
H16 H 0.621745 0.634864 0.670284 0.035 Uiso 1 1 calc R . . . .
C17 C 0.4656(3) 0.7824(2) 0.54487(16) 0.0211(9) Uani 1 1 d . . . . .
C18 C 0.4485(3) 0.8511(2) 0.53493(18) 0.0283(11) Uani 1 1 d . . . . .
C19 C 0.5172(4) 0.8824(2) 0.4985(2) 0.0442(13) Uani 1 1 d . . . . .
H19 H 0.508138 0.929285 0.490340 0.053 Uiso 1 1 calc R . . . .
C20 C 0.5980(4) 0.8469(3) 0.4741(2) 0.0503(15) Uani 1 1 d . . . . .
H20 H 0.644847 0.869485 0.449831 0.060 Uiso 1 1 calc R . . . .
C21 C 0.6113(3) 0.7785(3) 0.48461(19) 0.0410(13) Uani 1 1 d . . . . .
H21 H 0.666971 0.754445 0.467240 0.049 Uiso 1 1 calc R . . . .
C22 C 0.5444(3) 0.7442(2) 0.52030(17) 0.0278(11) Uani 1 1 d . . . . .
C23 C 0.3554(3) 0.8891(2) 0.55851(19) 0.0309(11) Uani 1 1 d . . . . .
H23 H 0.335469 0.865988 0.593603 0.037 Uiso 1 1 calc R . . . .
C24 C 0.2586(3) 0.8849(2) 0.5179(2) 0.0435(13) Uani 1 1 d . . . . .
H24A H 0.276904 0.905757 0.482600 0.065 Uiso 1 1 calc GR . . . .
H24B H 0.197908 0.908955 0.533552 0.065 Uiso 1 1 calc GR . . . .
H24C H 0.239471 0.837178 0.511816 0.065 Uiso 1 1 calc GR . . . .
C25 C 0.3802(4) 0.9632(2) 0.5723(2) 0.0465(14) Uani 1 1 d . . . . .
H25A H 0.448853 0.965957 0.592617 0.070 Uiso 1 1 calc GR . . . .
H25B H 0.323719 0.981755 0.595164 0.070 Uiso 1 1 calc GR . . . .
H25C H 0.384106 0.989413 0.537927 0.070 Uiso 1 1 calc GR . . . .
C26 C 0.5559(3) 0.6682(2) 0.52869(18) 0.0288(11) Uani 1 1 d . . . . .
H26 H 0.516496 0.655642 0.562659 0.035 Uiso 1 1 calc R . . . .
C27 C 0.6718(3) 0.6461(2) 0.53725(19) 0.0383(12) Uani 1 1 d . . . . .
H27A H 0.711091 0.655019 0.503464 0.057 Uiso 1 1 calc GR . . . .
H27B H 0.674303 0.597499 0.545674 0.057 Uiso 1 1 calc GR . . . .
H27C H 0.704383 0.671670 0.568114 0.057 Uiso 1 1 calc GR . . . .
C28 C 0.5038(4) 0.6309(2) 0.4797(2) 0.0467(14) Uani 1 1 d . . . . .
H28A H 0.430732 0.647542 0.473658 0.070 Uiso 1 1 calc GR . . . .
H28B H 0.502221 0.582106 0.487565 0.070 Uiso 1 1 calc GR . . . .
H28C H 0.545114 0.639022 0.446440 0.070 Uiso 1 1 calc GR . . . .
C29 C 0.5877(3) 0.83289(19) 0.82508(16) 0.0212(10) Uani 1 1 d . . . . .
C30 C 0.4948(3) 0.8584(2) 0.84795(17) 0.0260(10) Uani 1 1 d . . . . .
C31 C 0.4939(3) 0.9277(2) 0.85922(18) 0.0305(11) Uani 1 1 d . . . . .
H31 H 0.432448 0.947227 0.875105 0.037 Uiso 1 1 calc R . . . .
C32 C 0.5795(3) 0.9685(2) 0.84798(17) 0.0291(11) Uani 1 1 d . . . . .
H32 H 0.576284 1.015844 0.855389 0.035 Uiso 1 1 calc R . . . .
C33 C 0.6699(3) 0.9408(2) 0.82595(17) 0.0274(10) Uani 1 1 d . . . . .
H33 H 0.729139 0.969430 0.819011 0.033 Uiso 1 1 calc R . . . .
C34 C 0.6770(3) 0.87186(19) 0.81354(16) 0.0200(9) Uani 1 1 d . . . . .
C35 C 0.4000(3) 0.8147(2) 0.8616(2) 0.0377(12) Uani 1 1 d . . . . .
H35 H 0.408046 0.770338 0.841993 0.045 Uiso 1 1 calc R . . . .
C36 C 0.2932(3) 0.8456(3) 0.8429(2) 0.0546(16) Uani 1 1 d . . . . .
H36A H 0.278715 0.885869 0.865256 0.082 Uiso 1 1 calc GR . . . .
H36B H 0.236171 0.812204 0.847588 0.082 Uiso 1 1 calc GR . . . .
H36C H 0.296323 0.858517 0.803792 0.082 Uiso 1 1 calc GR . . . .
C37 C 0.4025(4) 0.8003(3) 0.9239(2) 0.0551(16) Uani 1 1 d . . . . .
H37A H 0.471527 0.780264 0.934795 0.083 Uiso 1 1 calc GR . . . .
H37B H 0.344991 0.768694 0.932680 0.083 Uiso 1 1 calc GR . . . .
H37C H 0.392635 0.842882 0.944159 0.083 Uiso 1 1 calc GR . . . .
C38 C 0.7777(3) 0.8432(2) 0.78889(17) 0.0221(10) Uani 1 1 d . . . . .
H38 H 0.758574 0.799779 0.769695 0.026 Uiso 1 1 calc R . . . .
C39 C 0.8584(3) 0.8269(2) 0.83558(18) 0.0350(12) Uani 1 1 d . . . . .
H39A H 0.876463 0.868587 0.855917 0.052 Uiso 1 1 calc GR . . . .
H39B H 0.923222 0.807813 0.819886 0.052 Uiso 1 1 calc GR . . . .
H39C H 0.827259 0.793942 0.860872 0.052 Uiso 1 1 calc GR . . . .
C40 C 0.8240(3) 0.8913(2) 0.74611(17) 0.0299(11) Uani 1 1 d . . . . .
H40A H 0.769299 0.901623 0.717592 0.045 Uiso 1 1 calc GR . . . .
H40B H 0.885399 0.869798 0.728919 0.045 Uiso 1 1 calc GR . . . .
H40C H 0.847000 0.933486 0.764373 0.045 Uiso 1 1 calc GR . . . .
C41 C 0.1468(3) 0.66985(19) 0.58885(16) 0.0182(9) Uani 1 1 d . . . . .
C42 C 0.0622(3) 0.70436(19) 0.61172(16) 0.0205(10) Uani 1 1 d . . . . .
C43 C -0.0397(3) 0.6772(2) 0.60032(18) 0.0272(11) Uani 1 1 d . . . . .
H43 H -0.100741 0.698536 0.615061 0.033 Uiso 1 1 calc R . . . .
C44 C -0.0524(3) 0.6199(2) 0.56808(19) 0.0340(12) Uani 1 1 d . . . . .
H44 H -0.122042 0.602344 0.560812 0.041 Uiso 1 1 calc R . . . .
C45 C 0.0351(3) 0.5878(2) 0.54620(18) 0.0310(11) Uani 1 1 d . . . . .
H45 H 0.024577 0.548456 0.524036 0.037 Uiso 1 1 calc R . . . .
C46 C 0.1378(3) 0.6119(2) 0.55591(16) 0.0217(9) Uani 1 1 d . . . . .
C47 C 0.0737(3) 0.76736(19) 0.64707(17) 0.0245(10) Uani 1 1 d . . . . .
H47 H 0.151572 0.778049 0.651195 0.029 Uiso 1 1 calc R . . . .
C48 C 0.0303(3) 0.7556(2) 0.70513(17) 0.0325(11) Uani 1 1 d . . . . .
H48A H -0.047350 0.749744 0.702530 0.049 Uiso 1 1 calc GR . . . .
H48B H 0.047610 0.794767 0.728679 0.049 Uiso 1 1 calc GR . . . .
H48C H 0.063068 0.714689 0.721255 0.049 Uiso 1 1 calc GR . . . .
C49 C 0.0182(4) 0.8284(2) 0.61920(19) 0.0369(12) Uani 1 1 d . . . . .
H49A H 0.046529 0.834967 0.582156 0.055 Uiso 1 1 calc GR . . . .
H49B H 0.031409 0.869206 0.641507 0.055 Uiso 1 1 calc GR . . . .
H49C H -0.058878 0.819909 0.616149 0.055 Uiso 1 1 calc GR . . . .
C50 C 0.2318(3) 0.5757(2) 0.53094(17) 0.0262(10) Uani 1 1 d . . . . .
H50 H 0.298237 0.599626 0.543894 0.031 Uiso 1 1 calc R . . . .
C51 C 0.2262(4) 0.5801(3) 0.46815(18) 0.0492(14) Uani 1 1 d . . . . .
H51A H 0.162264 0.556336 0.454143 0.074 Uiso 1 1 calc GR . . . .
H51B H 0.289919 0.558880 0.452945 0.074 Uiso 1 1 calc GR . . . .
H51C H 0.222912 0.627796 0.456856 0.074 Uiso 1 1 calc GR . . . .
C52 C 0.2402(4) 0.5020(2) 0.5505(2) 0.0430(13) Uani 1 1 d . . . . .
H52A H 0.244352 0.500754 0.591062 0.065 Uiso 1 1 calc GR . . . .
H52B H 0.304573 0.481222 0.535655 0.065 Uiso 1 1 calc GR . . . .
H52C H 0.177100 0.476693 0.537350 0.065 Uiso 1 1 calc GR . . . .
C53 C 0.6502(3) 0.59678(19) 0.85471(17) 0.0226(10) Uani 1 1 d . . . . .
C54 C 0.7548(3) 0.5765(2) 0.84283(16) 0.0241(10) Uani 1 1 d . . . . .
C55 C 0.7872(4) 0.5145(2) 0.86527(18) 0.0313(11) Uani 1 1 d . . . . .
H55 H 0.856512 0.497798 0.857673 0.038 Uiso 1 1 calc R . . . .
C56 C 0.7210(4) 0.4764(2) 0.89840(18) 0.0351(12) Uani 1 1 d . . . . .
H56 H 0.744235 0.433652 0.912345 0.042 Uiso 1 1 calc R . . . .
C57 C 0.6213(4) 0.5009(2) 0.91102(17) 0.0325(12) Uani 1 1 d . . . . .
H57 H 0.577812 0.475233 0.934908 0.039 Uiso 1 1 calc R . . . .
C58 C 0.5824(3) 0.5620(2) 0.88992(17) 0.0277(11) Uani 1 1 d . . . . .
C59 C 0.8298(3) 0.6195(2) 0.80962(17) 0.0264(10) Uani 1 1 d . . . . .
H59 H 0.791271 0.661988 0.798398 0.032 Uiso 1 1 calc R . . . .
C60 C 0.9272(3) 0.6395(2) 0.84630(19) 0.0366(12) Uani 1 1 d . . . . .
H60A H 0.903153 0.664247 0.878870 0.055 Uiso 1 1 calc GR . . . .
H60B H 0.974949 0.668476 0.825137 0.055 Uiso 1 1 calc GR . . . .
H60C H 0.965617 0.598460 0.858231 0.055 Uiso 1 1 calc GR . . . .
C61 C 0.8646(4) 0.5837(2) 0.75743(18) 0.0379(12) Uani 1 1 d . . . . .
H61A H 0.903894 0.542273 0.767524 0.057 Uiso 1 1 calc GR . . . .
H61B H 0.910909 0.613818 0.736477 0.057 Uiso 1 1 calc GR . . . .
H61C H 0.801523 0.571784 0.734603 0.057 Uiso 1 1 calc GR . . . .
C62 C 0.4758(3) 0.5911(2) 0.90670(18) 0.0335(12) Uani 1 1 d . . . . .
H62 H 0.452501 0.624637 0.877730 0.040 Uiso 1 1 calc R . . . .
C63 C 0.4895(4) 0.6292(3) 0.96130(19) 0.0460(14) Uani 1 1 d . . . . .
H63A H 0.514188 0.597643 0.990278 0.069 Uiso 1 1 calc GR . . . .
H63B H 0.420867 0.648837 0.971516 0.069 Uiso 1 1 calc GR . . . .
H63C H 0.542170 0.665480 0.957240 0.069 Uiso 1 1 calc GR . . . .
C64 C 0.3879(4) 0.5383(3) 0.9115(2) 0.0535(15) Uani 1 1 d . . . . .
H64A H 0.384128 0.510884 0.877626 0.080 Uiso 1 1 calc GR . . . .
H64B H 0.319303 0.561153 0.916486 0.080 Uiso 1 1 calc GR . . . .
H64C H 0.403613 0.508870 0.943335 0.080 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0617(4) 0.0308(3) 0.0450(3) -0.0129(2) -0.0193(3) 0.0208(3)
Br2 0.0177(2) 0.0436(3) 0.0280(3) -0.0052(2) 0.00284(19) -0.0085(2)
Co1 0.0144(3) 0.0199(3) 0.0213(3) -0.0017(3) -0.0018(2) -0.0004(2)
N1 0.0089(16) 0.0165(17) 0.022(2) 0.0027(15) 0.0003(15) -0.0003(14)
N2 0.0119(16) 0.0211(18) 0.0211(19) 0.0002(16) -0.0006(15) 0.0000(15)
N3 0.0123(17) 0.0146(17) 0.0192(19) 0.0011(15) 0.0024(15) 0.0002(14)
N4 0.0144(17) 0.0200(18) 0.019(2) -0.0027(15) 0.0023(15) -0.0015(14)
N5 0.0133(17) 0.0239(19) 0.0204(19) -0.0007(17) 0.0023(14) -0.0045(16)
N6 0.0178(18) 0.0221(19) 0.019(2) 0.0000(16) -0.0008(16) -0.0023(15)
C1 0.016(2) 0.017(2) 0.014(2) 0.0002(17) 0.0016(17) 0.0025(17)
C2 0.012(2) 0.013(2) 0.019(2) -0.0030(17) -0.0007(18) 0.0016(16)
C3 0.012(2) 0.024(2) 0.020(2) -0.0098(19) 0.0041(18) -0.0035(18)
C4 0.013(2) 0.022(2) 0.018(2) 0.0003(19) -0.0011(18) -0.0016(18)
C5 0.0068(19) 0.024(2) 0.022(2) 0.0029(19) 0.0008(18) 0.0015(17)
C6 0.019(2) 0.030(2) 0.023(3) -0.002(2) -0.001(2) -0.0017(19)
C7 0.021(2) 0.043(3) 0.018(3) 0.001(2) 0.000(2) 0.002(2)
C8 0.018(2) 0.048(3) 0.019(3) 0.014(2) 0.001(2) -0.002(2)
C9 0.015(2) 0.026(2) 0.037(3) 0.013(2) -0.003(2) -0.0011(19)
C10 0.015(2) 0.023(2) 0.023(2) 0.0018(19) -0.0068(19) 0.0038(18)
C11 0.018(2) 0.020(2) 0.023(3) 0.0004(19) -0.0084(19) 0.0060(18)
C12 0.019(2) 0.027(2) 0.035(3) 0.001(2) -0.006(2) 0.000(2)
C13 0.027(3) 0.017(2) 0.058(4) -0.001(2) -0.014(3) 0.003(2)
C14 0.040(3) 0.021(2) 0.041(3) -0.009(2) -0.019(3) 0.007(2)
C15 0.050(3) 0.029(3) 0.025(3) -0.006(2) -0.007(2) 0.012(2)
C16 0.037(3) 0.023(2) 0.028(3) -0.004(2) -0.006(2) 0.006(2)
C17 0.014(2) 0.032(2) 0.018(2) 0.006(2) 0.0002(18) -0.002(2)
C18 0.019(2) 0.036(3) 0.030(3) 0.006(2) -0.001(2) -0.004(2)
C19 0.036(3) 0.042(3) 0.055(4) 0.022(3) 0.009(3) -0.007(3)
C20 0.029(3) 0.070(4) 0.053(4) 0.028(3) 0.013(3) -0.008(3)
C21 0.021(2) 0.064(4) 0.038(3) 0.011(3) 0.011(2) 0.011(3)
C22 0.016(2) 0.047(3) 0.020(3) 0.004(2) 0.000(2) 0.000(2)
C23 0.027(2) 0.025(2) 0.041(3) 0.011(2) 0.000(2) -0.001(2)
C24 0.030(3) 0.038(3) 0.062(4) 0.016(3) -0.001(3) 0.002(2)
C25 0.041(3) 0.024(3) 0.075(4) 0.015(3) 0.002(3) -0.006(2)
C26 0.021(2) 0.037(3) 0.029(3) -0.007(2) 0.005(2) 0.006(2)
C27 0.026(3) 0.046(3) 0.043(3) -0.016(3) 0.000(2) 0.009(2)
C28 0.026(3) 0.061(3) 0.053(4) -0.013(3) -0.008(3) 0.001(2)
C29 0.024(2) 0.022(2) 0.017(2) -0.0069(19) -0.0010(19) 0.0002(19)
C30 0.023(2) 0.031(3) 0.024(3) -0.011(2) 0.002(2) -0.004(2)
C31 0.021(2) 0.039(3) 0.031(3) -0.012(2) 0.007(2) 0.005(2)
C32 0.036(3) 0.024(2) 0.027(3) -0.007(2) 0.002(2) 0.001(2)
C33 0.030(3) 0.025(2) 0.027(3) 0.002(2) 0.001(2) -0.006(2)
C34 0.024(2) 0.022(2) 0.014(2) -0.0036(18) -0.0009(19) -0.0019(19)
C35 0.024(2) 0.046(3) 0.044(3) -0.027(3) 0.013(2) -0.010(2)
C36 0.020(3) 0.063(4) 0.081(4) -0.038(3) 0.004(3) -0.001(3)
C37 0.046(3) 0.057(4) 0.063(4) -0.016(3) 0.030(3) -0.022(3)
C38 0.016(2) 0.023(2) 0.027(3) -0.005(2) 0.001(2) -0.0017(18)
C39 0.024(2) 0.039(3) 0.042(3) 0.000(2) 0.002(2) 0.002(2)
C40 0.026(2) 0.032(2) 0.032(3) -0.004(2) 0.005(2) -0.005(2)
C41 0.009(2) 0.024(2) 0.022(2) 0.0037(19) -0.0064(18) -0.0039(18)
C42 0.014(2) 0.025(2) 0.023(2) 0.0103(19) 0.0001(18) -0.0013(18)
C43 0.012(2) 0.035(3) 0.035(3) 0.007(2) 0.002(2) 0.005(2)
C44 0.022(2) 0.034(3) 0.045(3) 0.005(2) -0.013(2) -0.008(2)
C45 0.027(3) 0.029(3) 0.036(3) -0.001(2) -0.008(2) -0.007(2)
C46 0.019(2) 0.025(2) 0.021(2) -0.001(2) -0.0014(19) -0.0032(19)
C47 0.011(2) 0.026(2) 0.036(3) 0.003(2) 0.0036(19) 0.0040(18)
C48 0.028(3) 0.035(3) 0.034(3) -0.002(2) 0.006(2) 0.004(2)
C49 0.035(3) 0.027(3) 0.049(3) 0.011(2) 0.010(2) 0.007(2)
C50 0.021(2) 0.032(3) 0.026(3) -0.009(2) 0.001(2) -0.003(2)
C51 0.039(3) 0.079(4) 0.029(3) -0.009(3) 0.001(2) -0.015(3)
C52 0.043(3) 0.029(3) 0.057(4) -0.009(3) 0.011(3) 0.001(2)
C53 0.025(2) 0.021(2) 0.022(2) 0.0007(19) -0.007(2) -0.0041(19)
C54 0.025(2) 0.027(2) 0.020(2) -0.005(2) -0.004(2) -0.001(2)
C55 0.030(3) 0.031(3) 0.032(3) -0.002(2) -0.009(2) 0.001(2)
C56 0.044(3) 0.028(3) 0.033(3) 0.000(2) -0.013(2) 0.000(2)
C57 0.041(3) 0.033(3) 0.023(3) 0.010(2) -0.009(2) -0.015(2)
C58 0.024(2) 0.036(3) 0.022(3) 0.004(2) -0.011(2) -0.011(2)
C59 0.024(2) 0.026(2) 0.030(3) 0.000(2) 0.004(2) 0.002(2)
C60 0.026(3) 0.038(3) 0.045(3) 0.001(2) 0.000(2) -0.005(2)
C61 0.041(3) 0.040(3) 0.033(3) -0.001(2) 0.008(2) 0.002(2)
C62 0.020(2) 0.048(3) 0.032(3) 0.017(2) -0.003(2) -0.008(2)
C63 0.033(3) 0.071(4) 0.034(3) 0.004(3) 0.001(2) -0.002(3)
C64 0.032(3) 0.072(4) 0.056(4) 0.020(3) -0.005(3) -0.016(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Co1 2.4085(7) . ?
Br2 Co1 2.4156(7) . ?
Co1 C1 2.054(4) . ?
Co1 C3 2.045(4) . ?
N1 N2 1.336(4) . ?
N1 C1 1.372(4) . ?
N1 C17 1.463(5) . ?
N2 N3 1.325(4) . ?
N3 C2 1.380(5) . ?
N3 C41 1.456(4) . ?
N4 N5 1.341(4) . ?
N4 C3 1.374(5) . ?
N4 C29 1.466(5) . ?
N5 N6 1.324(4) . ?
N6 C4 1.373(5) . ?
N6 C53 1.458(5) . ?
C1 C2 1.401(5) . ?
C2 C5 1.474(5) . ?
C3 C4 1.393(5) . ?
C4 C11 1.479(5) . ?
C5 C6 1.391(5) . ?
C5 C10 1.389(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.387(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.383(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.376(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.387(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.397(5) . ?
C11 C16 1.384(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.387(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.380(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.387(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(6) . ?
C17 C22 1.386(5) . ?
C18 C19 1.391(6) . ?
C18 C23 1.510(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.377(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.380(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.392(6) . ?
C22 C26 1.518(6) . ?
C23 H23 1.0000 . ?
C23 C24 1.541(6) . ?
C23 C25 1.527(6) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 1.0000 . ?
C26 C27 1.523(5) . ?
C26 C28 1.525(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.395(5) . ?
C29 C34 1.391(5) . ?
C30 C31 1.392(6) . ?
C30 C35 1.510(6) . ?
C31 H31 0.9500 . ?
C31 C32 1.373(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.377(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.395(5) . ?
C34 C38 1.518(5) . ?
C35 H35 1.0000 . ?
C35 C36 1.527(6) . ?
C35 C37 1.531(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38 1.0000 . ?
C38 C39 1.529(5) . ?
C38 C40 1.528(5) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.386(5) . ?
C41 C46 1.395(5) . ?
C42 C43 1.405(5) . ?
C42 C47 1.511(5) . ?
C43 H43 0.9500 . ?
C43 C44 1.377(6) . ?
C44 H44 0.9500 . ?
C44 C45 1.382(6) . ?
C45 H45 0.9500 . ?
C45 C46 1.385(5) . ?
C46 C50 1.515(5) . ?
C47 H47 1.0000 . ?
C47 C48 1.535(5) . ?
C47 C49 1.536(5) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50 1.0000 . ?
C50 C51 1.519(6) . ?
C50 C52 1.530(6) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.406(5) . ?
C53 C58 1.397(5) . ?
C54 C55 1.394(6) . ?
C54 C59 1.511(6) . ?
C55 H55 0.9500 . ?
C55 C56 1.387(6) . ?
C56 H56 0.9500 . ?
C56 C57 1.381(6) . ?
C57 H57 0.9500 . ?
C57 C58 1.390(6) . ?
C58 C62 1.518(6) . ?
C59 H59 1.0000 . ?
C59 C60 1.541(6) . ?
C59 C61 1.519(5) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62 1.0000 . ?
C62 C63 1.523(6) . ?
C62 C64 1.522(6) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Co1 Br2 114.29(3) . . ?
C1 Co1 Br1 101.84(10) . . ?
C1 Co1 Br2 111.78(10) . . ?
C3 Co1 Br1 110.81(10) . . ?
C3 Co1 Br2 101.84(10) . . ?
C3 Co1 C1 116.82(15) . . ?
N2 N1 C1 116.6(3) . . ?
N2 N1 C17 114.5(3) . . ?
C1 N1 C17 128.8(3) . . ?
N3 N2 N1 102.6(3) . . ?
N2 N3 C2 112.3(3) . . ?
N2 N3 C41 117.3(3) . . ?
C2 N3 C41 130.2(3) . . ?
N5 N4 C3 116.1(3) . . ?
N5 N4 C29 117.0(3) . . ?
C3 N4 C29 126.8(3) . . ?
N6 N5 N4 102.5(3) . . ?
N5 N6 C4 112.4(3) . . ?
N5 N6 C53 119.6(3) . . ?
C4 N6 C53 127.5(3) . . ?
N1 C1 Co1 124.6(3) . . ?
N1 C1 C2 101.1(3) . . ?
C2 C1 Co1 133.1(3) . . ?
N3 C2 C1 107.3(3) . . ?
N3 C2 C5 121.2(3) . . ?
C1 C2 C5 131.4(3) . . ?
N4 C3 Co1 127.9(3) . . ?
N4 C3 C4 101.2(3) . . ?
C4 C3 Co1 130.2(3) . . ?
N6 C4 C3 107.7(3) . . ?
N6 C4 C11 123.3(3) . . ?
C3 C4 C11 128.8(4) . . ?
C6 C5 C2 120.0(3) . . ?
C10 C5 C2 120.9(4) . . ?
C10 C5 C6 119.1(4) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 C5 119.8(4) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.5(4) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.0(4) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.8(4) . . ?
C10 C9 H9 120.1 . . ?
C5 C10 H10 119.6 . . ?
C9 C10 C5 120.8(4) . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C4 120.9(4) . . ?
C16 C11 C4 120.0(4) . . ?
C16 C11 C12 118.8(4) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.7(4) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.3 . . ?
C13 C14 C15 119.4(4) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 121.1(4) . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 120.0(4) . . ?
C11 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C18 C17 N1 117.7(3) . . ?
C22 C17 N1 118.0(4) . . ?
C22 C17 C18 124.2(4) . . ?
C17 C18 C19 116.5(4) . . ?
C17 C18 C23 122.4(4) . . ?
C19 C18 C23 120.9(4) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 C18 121.3(4) . . ?
C20 C19 H19 119.4 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.2(4) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 119.5 . . ?
C20 C21 C22 121.1(4) . . ?
C22 C21 H21 119.5 . . ?
C17 C22 C21 116.6(4) . . ?
C17 C22 C26 123.0(4) . . ?
C21 C22 C26 120.3(4) . . ?
C18 C23 H23 107.8 . . ?
C18 C23 C24 109.6(4) . . ?
C18 C23 C25 113.7(4) . . ?
C24 C23 H23 107.8 . . ?
C25 C23 H23 107.8 . . ?
C25 C23 C24 110.1(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26 107.9 . . ?
C22 C26 C27 112.8(4) . . ?
C22 C26 C28 109.6(4) . . ?
C27 C26 H26 107.9 . . ?
C27 C26 C28 110.7(3) . . ?
C28 C26 H26 107.9 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N4 117.6(4) . . ?
C34 C29 N4 118.1(3) . . ?
C34 C29 C30 124.3(4) . . ?
C29 C30 C35 123.3(4) . . ?
C31 C30 C29 116.3(4) . . ?
C31 C30 C35 120.4(4) . . ?
C30 C31 H31 119.1 . . ?
C32 C31 C30 121.7(4) . . ?
C32 C31 H31 119.1 . . ?
C31 C32 H32 120.1 . . ?
C31 C32 C33 119.9(4) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 119.1 . . ?
C32 C33 C34 121.8(4) . . ?
C34 C33 H33 119.1 . . ?
C29 C34 C33 116.1(4) . . ?
C29 C34 C38 123.7(3) . . ?
C33 C34 C38 120.3(4) . . ?
C30 C35 H35 107.8 . . ?
C30 C35 C36 113.2(4) . . ?
C30 C35 C37 108.9(4) . . ?
C36 C35 H35 107.8 . . ?
C36 C35 C37 111.1(4) . . ?
C37 C35 H35 107.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C34 C38 H38 108.0 . . ?
C34 C38 C39 109.2(3) . . ?
C34 C38 C40 111.6(3) . . ?
C39 C38 H38 108.0 . . ?
C40 C38 H38 108.0 . . ?
C40 C38 C39 112.0(3) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 N3 117.8(3) . . ?
C42 C41 C46 125.3(3) . . ?
C46 C41 N3 116.9(3) . . ?
C41 C42 C43 115.8(4) . . ?
C41 C42 C47 124.4(3) . . ?
C43 C42 C47 119.8(4) . . ?
C42 C43 H43 119.5 . . ?
C44 C43 C42 121.0(4) . . ?
C44 C43 H43 119.5 . . ?
C43 C44 H44 119.7 . . ?
C43 C44 C45 120.6(4) . . ?
C45 C44 H44 119.7 . . ?
C44 C45 H45 119.3 . . ?
C44 C45 C46 121.4(4) . . ?
C46 C45 H45 119.3 . . ?
C41 C46 C50 124.1(3) . . ?
C45 C46 C41 115.9(4) . . ?
C45 C46 C50 119.9(4) . . ?
C42 C47 H47 107.9 . . ?
C42 C47 C48 111.2(3) . . ?
C42 C47 C49 111.1(3) . . ?
C48 C47 H47 107.9 . . ?
C48 C47 C49 110.6(3) . . ?
C49 C47 H47 107.9 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C46 C50 H50 107.6 . . ?
C46 C50 C51 110.8(4) . . ?
C46 C50 C52 111.9(3) . . ?
C51 C50 H50 107.6 . . ?
C51 C50 C52 111.3(4) . . ?
C52 C50 H50 107.6 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 N6 116.6(4) . . ?
C58 C53 N6 118.8(4) . . ?
C58 C53 C54 124.7(4) . . ?
C53 C54 C59 123.0(4) . . ?
C55 C54 C53 115.7(4) . . ?
C55 C54 C59 121.3(4) . . ?
C54 C55 H55 119.1 . . ?
C56 C55 C54 121.7(4) . . ?
C56 C55 H55 119.1 . . ?
C55 C56 H56 120.1 . . ?
C57 C56 C55 119.7(4) . . ?
C57 C56 H56 120.1 . . ?
C56 C57 H57 118.9 . . ?
C56 C57 C58 122.2(4) . . ?
C58 C57 H57 118.9 . . ?
C53 C58 C62 121.9(4) . . ?
C57 C58 C53 115.8(4) . . ?
C57 C58 C62 122.1(4) . . ?
C54 C59 H59 108.1 . . ?
C54 C59 C60 109.4(3) . . ?
C54 C59 C61 112.1(3) . . ?
C60 C59 H59 108.1 . . ?
C61 C59 H59 108.1 . . ?
C61 C59 C60 110.9(4) . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C58 C62 H62 107.8 . . ?
C58 C62 C63 109.7(4) . . ?
C58 C62 C64 113.9(4) . . ?
C63 C62 H62 107.8 . . ?
C64 C62 H62 107.8 . . ?
C64 C62 C63 109.6(4) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
_shelx_res_file
;
TITL cobr2mic2_a.res in P2(1)/n
cobr2mic2.res
created by SHELXL-2016/6 at 12:37:23 on 18-Oct-2019
REM Old TITL CoBr2MIC2 in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.202, Rweak 0.019, Alpha 0.068, Orientation as input
REM Formula found by SHELXT: C64 N6 Co Br2
CELL 0.71073 12.5223 19.704 24.1592 90 91.489 90
ZERR 4 0.0007 0.0011 0.0013 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Br Co N
UNIT 256 312 8 4 24
L.S. 4
PLAN 20
SIZE 0.02 0.11 0.18
TEMP -173.15
BOND $H
list 4
fmap 2
acta
SHEL 25 -3
REM
REM
REM
WGHT 0.033200 3.091800
FVAR 0.14238
BR1 3 0.445819 0.889682 0.704007 11.00000 0.06170 0.03077 =
0.04505 -0.01294 -0.01931 0.02080
BR2 3 0.693851 0.781692 0.645212 11.00000 0.01770 0.04355 =
0.02803 -0.00524 0.00284 -0.00851
CO1 4 0.521875 0.779316 0.688205 11.00000 0.01437 0.01992 =
0.02126 -0.00169 -0.00181 -0.00043
N1 5 0.393459 0.747841 0.582296 11.00000 0.00894 0.01655 =
0.02179 0.00271 0.00025 -0.00029
N2 5 0.302528 0.725967 0.558272 11.00000 0.01193 0.02105 =
0.02106 0.00019 -0.00061 0.00004
N3 5 0.254090 0.695842 0.599764 11.00000 0.01230 0.01464 =
0.01919 0.00114 0.00236 0.00022
N4 5 0.589764 0.760580 0.810946 11.00000 0.01440 0.01999 =
0.01926 -0.00269 0.00228 -0.00149
N5 5 0.622737 0.717569 0.850863 11.00000 0.01328 0.02394 =
0.02036 -0.00069 0.00225 -0.00450
N6 5 0.610429 0.657650 0.826701 11.00000 0.01783 0.02205 =
0.01910 0.00001 -0.00085 -0.00228
C1 1 0.407151 0.734911 0.637816 11.00000 0.01575 0.01709 =
0.01416 0.00024 0.00159 0.00246
C2 1 0.314049 0.698263 0.648480 11.00000 0.01232 0.01268 =
0.01892 -0.00301 -0.00073 0.00160
C3 1 0.557416 0.731657 0.761570 11.00000 0.01214 0.02406 =
0.02014 -0.00984 0.00413 -0.00347
C4 1 0.571192 0.662940 0.773269 11.00000 0.01346 0.02241 =
0.01830 0.00029 -0.00112 -0.00160
C5 1 0.276685 0.665671 0.699362 11.00000 0.00682 0.02378 =
0.02165 0.00290 0.00075 0.00152
C6 1 0.290691 0.698094 0.750174 11.00000 0.01915 0.02953 =
0.02320 -0.00180 -0.00096 -0.00171
AFIX 43
H6 2 0.325335 0.740947 0.752233 11.00000 -1.20000
AFIX 0
C7 1 0.253927 0.667682 0.797841 11.00000 0.02149 0.04328 =
0.01819 0.00128 0.00049 0.00185
AFIX 43
H7 2 0.263329 0.689947 0.832504 11.00000 -1.20000
AFIX 0
C8 1 0.203715 0.605228 0.795295 11.00000 0.01830 0.04794 =
0.01904 0.01446 0.00061 -0.00157
AFIX 43
H8 2 0.178662 0.584782 0.828119 11.00000 -1.20000
AFIX 0
C9 1 0.190030 0.572689 0.745229 11.00000 0.01474 0.02619 =
0.03674 0.01264 -0.00252 -0.00108
AFIX 43
H9 2 0.155128 0.529911 0.743365 11.00000 -1.20000
AFIX 0
C10 1 0.227359 0.602555 0.697501 11.00000 0.01527 0.02250 =
0.02272 0.00180 -0.00679 0.00378
AFIX 43
H10 2 0.219092 0.579557 0.663095 11.00000 -1.20000
AFIX 0
C11 1 0.543275 0.603539 0.738347 11.00000 0.01812 0.02044 =
0.02291 0.00044 -0.00844 0.00599
C12 1 0.476689 0.552383 0.757741 11.00000 0.01950 0.02653 =
0.03451 0.00143 -0.00550 0.00040
AFIX 43
H12 2 0.453524 0.553833 0.794856 11.00000 -1.20000
AFIX 0
C13 1 0.444014 0.499482 0.723402 11.00000 0.02710 0.01742 =
0.05835 -0.00117 -0.01419 0.00312
AFIX 43
H13 2 0.398977 0.464855 0.737083 11.00000 -1.20000
AFIX 0
C14 1 0.476936 0.497173 0.669383 11.00000 0.03950 0.02129 =
0.04124 -0.00875 -0.01871 0.00671
AFIX 43
H14 2 0.454335 0.461232 0.645630 11.00000 -1.20000
AFIX 0
C15 1 0.542989 0.547530 0.650153 11.00000 0.04978 0.02945 =
0.02486 -0.00601 -0.00684 0.01211
AFIX 43
H15 2 0.566019 0.545833 0.613021 11.00000 -1.20000
AFIX 0
C16 1 0.576300 0.600584 0.684166 11.00000 0.03679 0.02271 =
0.02800 -0.00390 -0.00644 0.00622
AFIX 43
H16 2 0.621745 0.634864 0.670284 11.00000 -1.20000
AFIX 0
C17 1 0.465644 0.782404 0.544872 11.00000 0.01404 0.03167 =
0.01771 0.00576 0.00025 -0.00231
C18 1 0.448484 0.851070 0.534930 11.00000 0.01852 0.03591 =
0.03025 0.00613 -0.00082 -0.00406
C19 1 0.517186 0.882441 0.498499 11.00000 0.03577 0.04232 =
0.05499 0.02242 0.00939 -0.00676
AFIX 43
H19 2 0.508138 0.929285 0.490340 11.00000 -1.20000
AFIX 0
C20 1 0.598022 0.846883 0.474055 11.00000 0.02893 0.06994 =
0.05252 0.02829 0.01309 -0.00752
AFIX 43
H20 2 0.644847 0.869485 0.449831 11.00000 -1.20000
AFIX 0
C21 1 0.611286 0.778513 0.484613 11.00000 0.02148 0.06431 =
0.03777 0.01083 0.01095 0.01054
AFIX 43
H21 2 0.666971 0.754445 0.467240 11.00000 -1.20000
AFIX 0
C22 1 0.544415 0.744247 0.520298 11.00000 0.01628 0.04725 =
0.01982 0.00358 -0.00011 -0.00042
C23 1 0.355384 0.889142 0.558513 11.00000 0.02709 0.02464 =
0.04099 0.01136 -0.00041 -0.00089
AFIX 13
H23 2 0.335469 0.865988 0.593603 11.00000 -1.20000
AFIX 0
C24 1 0.258606 0.884869 0.517925 11.00000 0.02982 0.03814 =
0.06236 0.01575 -0.00123 0.00198
AFIX 137
H24A 2 0.276904 0.905757 0.482600 11.00000 -1.50000
H24B 2 0.197908 0.908955 0.533552 11.00000 -1.50000
H24C 2 0.239471 0.837178 0.511816 11.00000 -1.50000
AFIX 0
C25 1 0.380242 0.963198 0.572289 11.00000 0.04094 0.02369 =
0.07484 0.01525 0.00227 -0.00571
AFIX 137
H25A 2 0.448853 0.965957 0.592617 11.00000 -1.50000
H25B 2 0.323719 0.981755 0.595164 11.00000 -1.50000
H25C 2 0.384106 0.989413 0.537927 11.00000 -1.50000
AFIX 0
C26 1 0.555945 0.668214 0.528689 11.00000 0.02059 0.03711 =
0.02901 -0.00674 0.00544 0.00584
AFIX 13
H26 2 0.516496 0.655642 0.562659 11.00000 -1.20000
AFIX 0
C27 1 0.671753 0.646132 0.537248 11.00000 0.02584 0.04594 =
0.04299 -0.01637 0.00049 0.00919
AFIX 137
H27A 2 0.711091 0.655019 0.503464 11.00000 -1.50000
H27B 2 0.674303 0.597499 0.545674 11.00000 -1.50000
H27C 2 0.704383 0.671670 0.568114 11.00000 -1.50000
AFIX 0
C28 1 0.503846 0.630884 0.479710 11.00000 0.02561 0.06102 =
0.05286 -0.01298 -0.00825 0.00138
AFIX 137
H28A 2 0.430732 0.647542 0.473658 11.00000 -1.50000
H28B 2 0.502221 0.582106 0.487565 11.00000 -1.50000
H28C 2 0.545114 0.639022 0.446440 11.00000 -1.50000
AFIX 0
C29 1 0.587688 0.832892 0.825083 11.00000 0.02445 0.02177 =
0.01744 -0.00689 -0.00102 0.00022
C30 1 0.494799 0.858420 0.847955 11.00000 0.02305 0.03085 =
0.02429 -0.01074 0.00165 -0.00417
C31 1 0.493887 0.927701 0.859223 11.00000 0.02149 0.03875 =
0.03144 -0.01211 0.00659 0.00486
AFIX 43
H31 2 0.432448 0.947227 0.875105 11.00000 -1.20000
AFIX 0
C32 1 0.579463 0.968546 0.847982 11.00000 0.03604 0.02381 =
0.02750 -0.00731 0.00213 0.00059
AFIX 43
H32 2 0.576284 1.015844 0.855389 11.00000 -1.20000
AFIX 0
C33 1 0.669918 0.940810 0.825949 11.00000 0.03048 0.02474 =
0.02687 0.00211 0.00108 -0.00580
AFIX 43
H33 2 0.729139 0.969430 0.819011 11.00000 -1.20000
AFIX 0
C34 1 0.676967 0.871862 0.813540 11.00000 0.02356 0.02237 =
0.01409 -0.00361 -0.00089 -0.00186
C35 1 0.400030 0.814654 0.861627 11.00000 0.02351 0.04638 =
0.04371 -0.02657 0.01340 -0.00951
AFIX 13
H35 2 0.408046 0.770338 0.841993 11.00000 -1.20000
AFIX 0
C36 1 0.293241 0.845582 0.842887 11.00000 0.02023 0.06278 =
0.08079 -0.03764 0.00425 -0.00129
AFIX 137
H36A 2 0.278715 0.885869 0.865256 11.00000 -1.50000
H36B 2 0.236171 0.812204 0.847588 11.00000 -1.50000
H36C 2 0.296323 0.858517 0.803792 11.00000 -1.50000
AFIX 0
C37 1 0.402520 0.800336 0.923917 11.00000 0.04636 0.05739 =
0.06315 -0.01592 0.03022 -0.02248
AFIX 137
H37A 2 0.471527 0.780264 0.934795 11.00000 -1.50000
H37B 2 0.344991 0.768694 0.932680 11.00000 -1.50000
H37C 2 0.392635 0.842882 0.944159 11.00000 -1.50000
AFIX 0
C38 1 0.777734 0.843235 0.788890 11.00000 0.01628 0.02278 =
0.02717 -0.00475 0.00104 -0.00167
AFIX 13
H38 2 0.758574 0.799779 0.769695 11.00000 -1.20000
AFIX 0
C39 1 0.858409 0.826931 0.835581 11.00000 0.02437 0.03875 =
0.04185 -0.00002 0.00168 0.00248
AFIX 137
H39A 2 0.876463 0.868587 0.855917 11.00000 -1.50000
H39B 2 0.923222 0.807813 0.819886 11.00000 -1.50000
H39C 2 0.827259 0.793942 0.860872 11.00000 -1.50000
AFIX 0
C40 1 0.824005 0.891348 0.746109 11.00000 0.02580 0.03223 =
0.03191 -0.00387 0.00520 -0.00468
AFIX 137
H40A 2 0.769299 0.901623 0.717592 11.00000 -1.50000
H40B 2 0.885399 0.869798 0.728919 11.00000 -1.50000
H40C 2 0.847000 0.933486 0.764373 11.00000 -1.50000
AFIX 0
C41 1 0.146794 0.669853 0.588855 11.00000 0.00861 0.02351 =
0.02205 0.00370 -0.00637 -0.00394
C42 1 0.062170 0.704363 0.611719 11.00000 0.01393 0.02452 =
0.02299 0.01029 0.00013 -0.00125
C43 1 -0.039714 0.677154 0.600319 11.00000 0.01215 0.03473 =
0.03485 0.00729 0.00188 0.00504
AFIX 43
H43 2 -0.100741 0.698536 0.615061 11.00000 -1.20000
AFIX 0
C44 1 -0.052444 0.619928 0.568082 11.00000 0.02177 0.03430 =
0.04529 0.00471 -0.01336 -0.00833
AFIX 43
H44 2 -0.122042 0.602344 0.560812 11.00000 -1.20000
AFIX 0
C45 1 0.035098 0.587835 0.546202 11.00000 0.02713 0.02926 =
0.03627 -0.00105 -0.00760 -0.00699
AFIX 43
H45 2 0.024577 0.548456 0.524036 11.00000 -1.20000
AFIX 0
C46 1 0.137808 0.611875 0.555912 11.00000 0.01909 0.02477 =
0.02110 -0.00052 -0.00143 -0.00316
C47 1 0.073707 0.767355 0.647070 11.00000 0.01137 0.02639 =
0.03601 0.00340 0.00362 0.00402
AFIX 13
H47 2 0.151572 0.778049 0.651195 11.00000 -1.20000
AFIX 0
C48 1 0.030339 0.755574 0.705131 11.00000 0.02847 0.03501 =
0.03440 -0.00183 0.00602 0.00420
AFIX 137
H48A 2 -0.047350 0.749744 0.702530 11.00000 -1.50000
H48B 2 0.047610 0.794767 0.728679 11.00000 -1.50000
H48C 2 0.063068 0.714689 0.721255 11.00000 -1.50000
AFIX 0
C49 1 0.018167 0.828380 0.619199 11.00000 0.03532 0.02723 =
0.04876 0.01057 0.01038 0.00729
AFIX 137
H49A 2 0.046529 0.834967 0.582156 11.00000 -1.50000
H49B 2 0.031409 0.869206 0.641507 11.00000 -1.50000
H49C 2 -0.058878 0.819909 0.616149 11.00000 -1.50000
AFIX 0
C50 1 0.231784 0.575651 0.530944 11.00000 0.02110 0.03196 =
0.02552 -0.00891 0.00086 -0.00270
AFIX 13
H50 2 0.298237 0.599626 0.543894 11.00000 -1.20000
AFIX 0
C51 1 0.226227 0.580057 0.468149 11.00000 0.03886 0.07938 =
0.02945 -0.00925 0.00095 -0.01466
AFIX 137
H51A 2 0.162264 0.556336 0.454143 11.00000 -1.50000
H51B 2 0.289919 0.558880 0.452945 11.00000 -1.50000
H51C 2 0.222912 0.627796 0.456856 11.00000 -1.50000
AFIX 0
C52 1 0.240209 0.501958 0.550511 11.00000 0.04334 0.02901 =
0.05718 -0.00945 0.01115 0.00079
AFIX 137
H52A 2 0.244352 0.500754 0.591062 11.00000 -1.50000
H52B 2 0.304573 0.481222 0.535655 11.00000 -1.50000
H52C 2 0.177100 0.476693 0.537350 11.00000 -1.50000
AFIX 0
C53 1 0.650158 0.596784 0.854714 11.00000 0.02451 0.02109 =
0.02176 0.00071 -0.00750 -0.00414
C54 1 0.754769 0.576529 0.842834 11.00000 0.02503 0.02750 =
0.01952 -0.00481 -0.00421 -0.00065
C55 1 0.787233 0.514470 0.865270 11.00000 0.03030 0.03132 =
0.03163 -0.00169 -0.00905 0.00091
AFIX 43
H55 2 0.856512 0.497798 0.857673 11.00000 -1.20000
AFIX 0
C56 1 0.721037 0.476407 0.898401 11.00000 0.04369 0.02818 =
0.03253 -0.00035 -0.01350 -0.00043
AFIX 43
H56 2 0.744235 0.433652 0.912345 11.00000 -1.20000
AFIX 0
C57 1 0.621297 0.500939 0.911018 11.00000 0.04059 0.03339 =
0.02303 0.00986 -0.00872 -0.01471
AFIX 43
H57 2 0.577812 0.475233 0.934908 11.00000 -1.20000
AFIX 0
C58 1 0.582427 0.561991 0.889922 11.00000 0.02445 0.03610 =
0.02193 0.00438 -0.01077 -0.01055
C59 1 0.829779 0.619502 0.809616 11.00000 0.02415 0.02558 =
0.02965 -0.00017 0.00387 0.00249
AFIX 13
H59 2 0.791271 0.661988 0.798398 11.00000 -1.20000
AFIX 0
C60 1 0.927242 0.639490 0.846302 11.00000 0.02579 0.03849 =
0.04538 0.00119 -0.00002 -0.00518
AFIX 137
H60A 2 0.903153 0.664247 0.878870 11.00000 -1.50000
H60B 2 0.974949 0.668476 0.825137 11.00000 -1.50000
H60C 2 0.965617 0.598460 0.858231 11.00000 -1.50000
AFIX 0
C61 1 0.864617 0.583665 0.757425 11.00000 0.04059 0.04007 =
0.03333 -0.00126 0.00793 0.00221
AFIX 137
H61A 2 0.903894 0.542273 0.767524 11.00000 -1.50000
H61B 2 0.910909 0.613818 0.736477 11.00000 -1.50000
H61C 2 0.801523 0.571784 0.734603 11.00000 -1.50000
AFIX 0
C62 1 0.475819 0.591142 0.906697 11.00000 0.02008 0.04830 =
0.03199 0.01719 -0.00281 -0.00833
AFIX 13
H62 2 0.452501 0.624637 0.877730 11.00000 -1.20000
AFIX 0
C63 1 0.489478 0.629164 0.961298 11.00000 0.03332 0.07091 =
0.03385 0.00350 0.00062 -0.00162
AFIX 137
H63A 2 0.514188 0.597643 0.990278 11.00000 -1.50000
H63B 2 0.420867 0.648837 0.971516 11.00000 -1.50000
H63C 2 0.542170 0.665480 0.957240 11.00000 -1.50000
AFIX 0
C64 1 0.387889 0.538310 0.911460 11.00000 0.03159 0.07211 =
0.05635 0.01997 -0.00517 -0.01622
AFIX 137
H64A 2 0.384128 0.510884 0.877626 11.00000 -1.50000
H64B 2 0.319303 0.561153 0.916486 11.00000 -1.50000
H64C 2 0.403613 0.508870 0.943335 11.00000 -1.50000
AFIX 0
HKLF 4
REM cobr2mic2_a.res in P2(1)/n
REM R1 = 0.0509 for 6531 Fo > 4sig(Fo) and 0.1206 for all 11339 data
REM 674 parameters refined using 0 restraints
END
WGHT 0.0333 3.0732
REM Highest difference peak 0.690, deepest hole -0.777, 1-sigma level 0.087
Q1 1 0.6968 0.8647 0.4332 11.00000 0.05 0.69
Q2 1 0.7508 0.4191 0.9386 11.00000 0.05 0.69
Q3 1 0.5845 1.0444 0.8720 11.00000 0.05 0.61
Q4 1 0.3968 0.8596 0.7125 11.00000 0.05 0.57
Q5 1 -0.1725 0.5814 0.5932 11.00000 0.05 0.43
Q6 1 0.4780 0.8762 0.6905 11.00000 0.05 0.38
Q7 1 0.7266 0.7765 0.6896 11.00000 0.05 0.37
Q8 1 0.4413 0.9175 0.6990 11.00000 0.05 0.35
Q9 1 0.1247 0.6578 0.5528 11.00000 0.05 0.34
Q10 1 0.7286 0.3652 0.9096 11.00000 0.05 0.34
Q11 1 0.4028 0.7815 0.8252 11.00000 0.05 0.33
Q12 1 0.5294 0.6374 0.7685 11.00000 0.05 0.33
Q13 1 0.5242 0.9251 0.6638 11.00000 0.05 0.32
Q14 1 0.2411 0.6984 0.7262 11.00000 0.05 0.32
Q15 1 0.7227 0.8418 0.6345 11.00000 0.05 0.32
Q16 1 0.4627 0.8830 0.7445 11.00000 0.05 0.32
Q17 1 0.7638 0.5347 0.7378 11.00000 0.05 0.32
Q18 1 0.4590 0.7870 0.6479 11.00000 0.05 0.32
Q19 1 0.6384 0.8772 0.5200 11.00000 0.05 0.32
Q20 1 0.7464 0.3975 0.8738 11.00000 0.05 0.32
;
_shelx_res_checksum 83902
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_chemical_properties_physical Moisture-sensitive
_exptl_crystal_preparation 'Magnetic properties'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_jr204
_database_code_depnum_ccdc_archive 'CCDC 1960248'
loop_
_audit_author_name
_audit_author_address
'Milan Gembicky'
;University of California, San Diego
United States of America
;
_audit_update_record
;
2019-10-18 deposited with the CCDC. 2020-02-06 downloaded from the CCDC.
;
_audit_creation_date 2019-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic
'(1,3-bis(2,6-diisopropylphenyl)-5-phenyl-2,3-dihydro-1H-1,2,3-triazol-4-yl)(1-(2,6-diisopropylphenyl)-3-(2-ethyl-6-isopropylphenyl)-5-phenyl-2,3-dihydro-1H-1,2,3-triazol-4-yl)cobalt(II) iodide'
_chemical_formula_moiety 'C64 H78 Co I2 N6, C4 H8 O'
_chemical_formula_sum 'C68 H86 Co I2 N6 O'
_chemical_formula_weight 1316.15
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 56
_space_group_name_H-M_alt 'P c c n'
_space_group_name_Hall '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'
_cell_length_a 17.2279(5)
_cell_length_b 17.4336(5)
_cell_length_c 20.9343(6)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 6287.5(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9910
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 25.63
_cell_measurement_theta_min 2.27
_shelx_estimated_absorpt_T_max 0.981
_shelx_estimated_absorpt_T_min 0.938
_exptl_absorpt_coefficient_mu 1.301
_exptl_absorpt_correction_T_max 0.4906
_exptl_absorpt_correction_T_min 0.3940
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0784 before and 0.0566 after correction. The Ratio of minimum to maximum transmission is 0.7834. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear green'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary green
_exptl_crystal_density_diffrn 1.390
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description trapezoid
_exptl_crystal_F_000 2708
_exptl_crystal_preparation
'2 equiv free MIC with CoI2 in THF,Magnetic properties'
_exptl_crystal_recrystallization_method 'Concentrated THF room temp'
_exptl_crystal_size_max 0.05
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.015
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0596
_diffrn_reflns_av_unetI/netI 0.0356
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 52120
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.684
_diffrn_reflns_theta_min 1.182
_diffrn_ambient_temperature 100.0
_diffrn_detector 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device 'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type 'Bruker APEX II Ultra'
_diffrn_measurement_method '\w and \f scans'
_diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe X-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Micro Focus Rotating Anode'
_diffrn_source_type 'Bruker TXS'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4809
_reflns_number_total 5958
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection 'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction 'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.126
_refine_diff_density_min -0.721
_refine_diff_density_rms 0.091
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 384
_refine_ls_number_reflns 5958
_refine_ls_number_restraints 34
_refine_ls_R_factor_all 0.0609
_refine_ls_R_factor_gt 0.0407
_refine_ls_restrained_S_all 1.026
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+32.3712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0947
_refine_ls_wR_factor_ref 0.1084
_refine_special_details
;
Refined as a 2-component twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.9178(7)
0.0822(7)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
3. Restrained distances
O1S-C4S \\sim O1S-C1S
with sigma of 0.02
C3S-C4S \\sim C3S-C2S \\sim C1S-C2S
with sigma of 0.02
4. Rigid body (RIGU) restrains
O1S, C1S, C2S, C3S, C4S
with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
5. Others
Fixed Sof: O1S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5)
C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5)
6.a Ternary CH refined with riding coordinates:
C15(H15), C18(H18), C27(H27), C30(H30)
6.b Secondary CH2 refined with riding coordinates:
C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB)
6.c Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
C23(H23), C24(H24), C25(H25)
6.d Idealised Me refined as rotating group:
C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
H20C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,
H32B,H32C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.34695(2) 0.82259(2) 0.09101(2) 0.02667(11) Uani 1 1 d . . . . .
Co1 Co 0.2500 0.7500 0.16521(4) 0.01592(19) Uani 1 2 d S T P . .
N1 N 0.3634(2) 0.6173(2) 0.20374(16) 0.0180(8) Uani 1 1 d . . . . .
N2 N 0.4180(2) 0.5937(2) 0.24543(17) 0.0184(8) Uani 1 1 d . . . . .
N3 N 0.4152(2) 0.6480(2) 0.29004(17) 0.0171(8) Uani 1 1 d . . . . .
C1 C 0.3263(3) 0.6837(3) 0.2194(2) 0.0158(9) Uani 1 1 d . . . . .
C2 C 0.3602(3) 0.7022(3) 0.2775(2) 0.0178(10) Uani 1 1 d . . . . .
C3 C 0.3488(3) 0.7681(3) 0.3208(2) 0.0184(10) Uani 1 1 d . . . . .
C4 C 0.3463(3) 0.8417(3) 0.2955(2) 0.0207(10) Uani 1 1 d . . . . .
H4 H 0.3510 0.8491 0.2507 0.025 Uiso 1 1 calc R . . . .
C5 C 0.3369(3) 0.9046(3) 0.3354(2) 0.0272(12) Uani 1 1 d . . . . .
H5 H 0.3359 0.9549 0.3180 0.033 Uiso 1 1 calc R . . . .
C6 C 0.3289(3) 0.8940(3) 0.4010(2) 0.0273(12) Uani 1 1 d . . . . .
H6 H 0.3220 0.9370 0.4283 0.033 Uiso 1 1 calc R . . . .
C7 C 0.3311(3) 0.8210(3) 0.4265(2) 0.0242(11) Uani 1 1 d . . . . .
H7 H 0.3258 0.8139 0.4713 0.029 Uiso 1 1 calc R . . . .
C8 C 0.3411(3) 0.7577(3) 0.3867(2) 0.0202(10) Uani 1 1 d . . . . .
H8 H 0.3426 0.7075 0.4043 0.024 Uiso 1 1 calc R . . . .
C9 C 0.4688(3) 0.6460(3) 0.3439(2) 0.0192(10) Uani 1 1 d . . . . .
C10 C 0.5263(3) 0.7023(3) 0.3475(2) 0.0213(11) Uani 1 1 d . . . . .
C11 C 0.5720(3) 0.7028(3) 0.4026(2) 0.0272(12) Uani 1 1 d . . . . .
H11 H 0.6125 0.7394 0.4067 0.033 Uiso 1 1 calc R . . . .
C12 C 0.5591(3) 0.6512(3) 0.4512(3) 0.0301(13) Uani 1 1 d . . . . .
H12 H 0.5901 0.6533 0.4887 0.036 Uiso 1 1 calc R . . . .
C13 C 0.5017(3) 0.5965(3) 0.4462(2) 0.0274(12) Uani 1 1 d . . . . .
H13 H 0.4940 0.5615 0.4804 0.033 Uiso 1 1 calc R . . . .
C14 C 0.4547(3) 0.5913(3) 0.3919(2) 0.0206(10) Uani 1 1 d . . . . .
C15 C 0.5418(3) 0.7605(3) 0.2950(2) 0.0252(11) Uani 1 1 d . . . . .
H15 H 0.4979 0.7580 0.2638 0.030 Uiso 1 1 calc R . . . .
C16 C 0.6169(3) 0.7407(4) 0.2593(3) 0.0368(13) Uani 1 1 d . . . . .
H16A H 0.6605 0.7405 0.2894 0.055 Uiso 1 1 calc GR . . . .
H16B H 0.6263 0.7790 0.2259 0.055 Uiso 1 1 calc GR . . . .
H16C H 0.6119 0.6899 0.2397 0.055 Uiso 1 1 calc GR . . . .
C17 C 0.5458(3) 0.8424(3) 0.3216(3) 0.0316(13) Uani 1 1 d . . . . .
H17A H 0.4986 0.8532 0.3462 0.047 Uiso 1 1 calc GR . . . .
H17B H 0.5499 0.8789 0.2862 0.047 Uiso 1 1 calc GR . . . .
H17C H 0.5913 0.8474 0.3494 0.047 Uiso 1 1 calc GR . . . .
C18 C 0.3945(3) 0.5287(3) 0.3863(2) 0.0222(11) Uani 1 1 d . . . . .
H18 H 0.3570 0.5442 0.3522 0.027 Uiso 1 1 calc R . . . .
C19 C 0.4339(3) 0.4542(3) 0.3647(2) 0.0278(12) Uani 1 1 d . . . . .
H19A H 0.4589 0.4623 0.3233 0.042 Uiso 1 1 calc GR . . . .
H19B H 0.3948 0.4135 0.3608 0.042 Uiso 1 1 calc GR . . . .
H19C H 0.4730 0.4391 0.3963 0.042 Uiso 1 1 calc GR . . . .
C20 C 0.3481(3) 0.5158(3) 0.4479(2) 0.0281(11) Uani 1 1 d . . . . .
H20A H 0.3822 0.4941 0.4807 0.042 Uiso 1 1 calc GR . . . .
H20B H 0.3052 0.4803 0.4395 0.042 Uiso 1 1 calc GR . . . .
H20C H 0.3272 0.5649 0.4629 0.042 Uiso 1 1 calc GR . . . .
C21 C 0.3550(3) 0.5695(3) 0.1470(2) 0.0176(10) Uani 1 1 d . . . . .
C22 C 0.4109(3) 0.5777(3) 0.0988(2) 0.0190(10) Uani 1 1 d . . . . .
C23 C 0.4023(3) 0.5309(3) 0.0453(2) 0.0232(11) Uani 1 1 d . . . . .
H23 H 0.4389 0.5347 0.0115 0.028 Uiso 1 1 calc R . . . .
C24 C 0.3424(3) 0.4795(3) 0.0402(2) 0.0248(11) Uani 1 1 d . . . . .
H24 H 0.3377 0.4486 0.0031 0.030 Uiso 1 1 calc R . . . .
C25 C 0.2885(3) 0.4725(3) 0.0893(2) 0.0227(10) Uani 1 1 d . . . . .
H25 H 0.2473 0.4366 0.0854 0.027 Uiso 1 1 calc R . . . .
C26 C 0.2940(3) 0.5175(3) 0.1440(2) 0.0206(10) Uani 1 1 d . . . . .
C27 C 0.4815(3) 0.6299(3) 0.1049(2) 0.0215(10) Uani 1 1 d . . . . .
H27 H 0.4690 0.6700 0.1374 0.026 Uiso 1 1 calc R . . . .
C28 C 0.5508(3) 0.5834(3) 0.1301(2) 0.0293(12) Uani 1 1 d . . . . .
H28A H 0.5378 0.5616 0.1719 0.044 Uiso 1 1 calc GR . . . .
H28B H 0.5960 0.6170 0.1343 0.044 Uiso 1 1 calc GR . . . .
H28C H 0.5627 0.5418 0.1001 0.044 Uiso 1 1 calc GR . . . .
C29 C 0.5037(3) 0.6712(3) 0.0427(2) 0.0290(12) Uani 1 1 d . . . . .
H29A H 0.5222 0.6335 0.0114 0.043 Uiso 1 1 calc GR . . . .
H29B H 0.5449 0.7085 0.0514 0.043 Uiso 1 1 calc GR . . . .
H29C H 0.4581 0.6978 0.0256 0.043 Uiso 1 1 calc GR . . . .
C30 C 0.2391(3) 0.5044(3) 0.2000(2) 0.0221(11) Uani 1 1 d . . . . .
H30 H 0.2355 0.5537 0.2243 0.027 Uiso 1 1 calc R . . . .
C31 C 0.2739(3) 0.4439(3) 0.2448(2) 0.0274(12) Uani 1 1 d . . . . .
H31A H 0.2757 0.3942 0.2229 0.041 Uiso 1 1 calc GR . . . .
H31B H 0.2417 0.4396 0.2832 0.041 Uiso 1 1 calc GR . . . .
H31C H 0.3266 0.4592 0.2569 0.041 Uiso 1 1 calc GR . . . .
C32 C 0.1561(3) 0.4812(3) 0.1803(3) 0.0303(12) Uani 1 1 d . . . . .
H32A H 0.1358 0.5184 0.1495 0.045 Uiso 1 1 calc GR . . . .
H32B H 0.1227 0.4803 0.2182 0.045 Uiso 1 1 calc GR . . . .
H32C H 0.1572 0.4301 0.1608 0.045 Uiso 1 1 calc GR . . . .
O1S O 0.2532(7) 0.3356(5) 0.4456(4) 0.055(3) Uani 0.5 1 d D U . A -1
C1S C 0.2681(17) 0.2862(10) 0.3922(9) 0.053(4) Uani 0.5 1 d D U . A -1
H1SA H 0.3243 0.2862 0.3823 0.063 Uiso 0.5 1 calc R . . A -1
H1SB H 0.2398 0.3051 0.3541 0.063 Uiso 0.5 1 calc R . . A -1
C2S C 0.2420(16) 0.2064(12) 0.4081(7) 0.054(5) Uani 0.5 1 d D U . A -1
H2SA H 0.2746 0.1671 0.3869 0.065 Uiso 0.5 1 calc R . . A -1
H2SB H 0.1869 0.1980 0.3967 0.065 Uiso 0.5 1 calc R . . A -1
C3S C 0.2541(12) 0.2068(10) 0.4803(6) 0.041(4) Uani 0.5 1 d D U . A -1
H3SA H 0.2204 0.1685 0.5016 0.049 Uiso 0.5 1 calc R . . A -1
H3SB H 0.3089 0.1963 0.4915 0.049 Uiso 0.5 1 calc R . . A -1
C4S C 0.2312(13) 0.2872(9) 0.4985(9) 0.041(3) Uani 0.5 1 d D U . A -1
H4SA H 0.1746 0.2903 0.5061 0.049 Uiso 0.5 1 calc R . . A -1
H4SB H 0.2585 0.3032 0.5379 0.049 Uiso 0.5 1 calc R . . A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0339(2) 0.02366(17) 0.02243(16) 0.00322(13) 0.00898(14) 0.00031(16)
Co1 0.0204(5) 0.0162(4) 0.0111(4) 0.000 0.000 0.0024(4)
N1 0.024(2) 0.018(2) 0.0117(17) 0.0002(15) -0.0011(16) -0.0008(17)
N2 0.022(2) 0.020(2) 0.0136(17) -0.0011(15) -0.0034(16) 0.0036(17)
N3 0.019(2) 0.019(2) 0.0131(18) -0.0013(15) -0.0013(16) 0.0009(16)
C1 0.022(2) 0.012(2) 0.014(2) -0.0031(18) 0.0047(17) -0.0054(18)
C2 0.024(3) 0.017(2) 0.013(2) 0.0042(17) 0.0027(19) 0.0012(19)
C3 0.016(2) 0.024(3) 0.015(2) -0.0013(18) -0.0021(19) 0.003(2)
C4 0.021(2) 0.026(3) 0.015(2) -0.0013(18) -0.004(2) 0.003(2)
C5 0.033(3) 0.021(3) 0.028(3) -0.002(2) -0.011(2) 0.002(2)
C6 0.029(3) 0.026(3) 0.027(3) -0.014(2) -0.005(2) 0.003(2)
C7 0.023(3) 0.033(3) 0.016(2) -0.007(2) -0.0019(18) 0.006(2)
C8 0.021(3) 0.021(2) 0.018(2) -0.0015(19) -0.004(2) 0.004(2)
C9 0.022(3) 0.021(2) 0.015(2) -0.0027(18) -0.0042(19) 0.007(2)
C10 0.024(3) 0.019(2) 0.020(2) -0.0014(19) 0.000(2) 0.005(2)
C11 0.031(3) 0.025(3) 0.025(3) -0.004(2) -0.010(2) -0.003(2)
C12 0.037(3) 0.029(3) 0.025(3) -0.001(2) -0.013(2) 0.005(2)
C13 0.036(3) 0.027(3) 0.019(2) 0.002(2) -0.010(2) 0.006(2)
C14 0.028(3) 0.020(2) 0.014(2) -0.0010(18) -0.0024(19) 0.005(2)
C15 0.026(3) 0.026(3) 0.024(2) 0.001(2) -0.001(2) -0.005(2)
C16 0.037(3) 0.040(3) 0.033(3) -0.003(3) 0.006(3) -0.004(3)
C17 0.031(3) 0.030(3) 0.034(3) 0.003(2) -0.001(2) -0.005(2)
C18 0.027(3) 0.024(3) 0.016(2) 0.0030(19) -0.004(2) 0.001(2)
C19 0.033(3) 0.027(3) 0.023(3) 0.000(2) -0.003(2) -0.002(2)
C20 0.032(3) 0.032(3) 0.021(2) 0.004(2) 0.001(2) 0.005(3)
C21 0.024(3) 0.015(2) 0.015(2) -0.0032(17) 0.0003(19) 0.004(2)
C22 0.024(3) 0.017(2) 0.016(2) 0.0033(18) -0.0002(19) 0.005(2)
C23 0.029(3) 0.023(3) 0.017(2) -0.001(2) 0.000(2) 0.009(2)
C24 0.038(3) 0.023(3) 0.013(2) -0.0017(19) -0.004(2) 0.009(2)
C25 0.033(3) 0.016(2) 0.019(2) -0.0010(19) -0.004(2) 0.002(2)
C26 0.025(3) 0.017(2) 0.020(2) -0.0020(19) -0.002(2) 0.007(2)
C27 0.022(3) 0.024(3) 0.019(2) -0.0025(19) 0.004(2) 0.000(2)
C28 0.023(3) 0.044(3) 0.021(2) 0.000(2) 0.001(2) 0.004(2)
C29 0.031(3) 0.036(3) 0.019(2) 0.004(2) 0.005(2) -0.001(3)
C30 0.027(3) 0.016(2) 0.023(2) 0.0009(19) -0.001(2) 0.000(2)
C31 0.034(3) 0.027(3) 0.022(2) 0.001(2) 0.001(2) 0.003(2)
C32 0.029(3) 0.028(3) 0.033(3) 0.004(2) 0.001(2) -0.001(2)
O1S 0.087(7) 0.031(4) 0.047(5) 0.005(4) 0.024(5) 0.001(4)
C1S 0.077(11) 0.038(5) 0.043(6) 0.002(4) 0.014(6) 0.011(5)
C2S 0.078(13) 0.041(5) 0.044(8) 0.007(4) -0.001(6) 0.006(6)
C3S 0.043(10) 0.037(4) 0.043(8) 0.008(4) 0.003(6) 0.003(4)
C4S 0.043(9) 0.036(4) 0.043(6) 0.010(4) 0.008(5) 0.003(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Co1 2.6084(6) . ?
Co1 I1 2.6084(6) 2_565 ?
Co1 C1 2.086(5) . ?
Co1 C1 2.086(5) 2_565 ?
N1 N2 1.347(5) . ?
N1 C1 1.363(6) . ?
N1 C21 1.458(5) . ?
N2 N3 1.331(5) . ?
N3 C2 1.363(6) . ?
N3 C9 1.458(6) . ?
C1 C2 1.387(6) . ?
C2 C3 1.477(6) . ?
C3 C4 1.389(7) . ?
C3 C8 1.398(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.395(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.397(7) . ?
C9 C14 1.406(7) . ?
C10 C11 1.397(7) . ?
C10 C15 1.519(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.375(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.377(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.399(7) . ?
C14 C18 1.511(7) . ?
C15 H15 1.0000 . ?
C15 C16 1.533(8) . ?
C15 C17 1.534(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 1.0000 . ?
C18 C19 1.533(7) . ?
C18 C20 1.533(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.402(6) . ?
C21 C26 1.389(7) . ?
C22 C23 1.394(6) . ?
C22 C27 1.524(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.370(7) . ?
C24 H24 0.9500 . ?
C24 C25 1.390(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.392(6) . ?
C26 C30 1.522(7) . ?
C27 H27 1.0000 . ?
C27 C28 1.536(7) . ?
C27 C29 1.536(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30 1.0000 . ?
C30 C31 1.535(7) . ?
C30 C32 1.542(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O1S C1S 1.435(15) . ?
O1S C4S 1.443(14) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C1S C2S 1.501(12) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C2S C3S 1.525(15) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C3S C4S 1.505(12) . ?
C4S H4SA 0.9900 . ?
C4S H4SB 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Co1 I1 106.91(3) 2_565 . ?
C1 Co1 I1 100.93(12) 2_565 2_565 ?
C1 Co1 I1 117.27(12) . 2_565 ?
C1 Co1 I1 117.27(12) 2_565 . ?
C1 Co1 I1 100.93(12) . . ?
C1 Co1 C1 114.1(2) 2_565 . ?
N2 N1 C1 115.5(4) . . ?
N2 N1 C21 115.1(4) . . ?
C1 N1 C21 129.4(4) . . ?
N3 N2 N1 102.2(3) . . ?
N2 N3 C2 112.5(4) . . ?
N2 N3 C9 120.1(4) . . ?
C2 N3 C9 127.3(4) . . ?
N1 C1 Co1 129.5(3) . . ?
N1 C1 C2 102.2(4) . . ?
C2 C1 Co1 127.8(3) . . ?
N3 C2 C1 107.5(4) . . ?
N3 C2 C3 120.8(4) . . ?
C1 C2 C3 131.6(4) . . ?
C4 C3 C2 119.3(4) . . ?
C4 C3 C8 119.6(4) . . ?
C8 C3 C2 121.1(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0(5) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.1(5) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.2(4) . . ?
C8 C7 H7 119.9 . . ?
C3 C8 H8 120.0 . . ?
C7 C8 C3 119.9(5) . . ?
C7 C8 H8 120.0 . . ?
C10 C9 N3 118.3(4) . . ?
C10 C9 C14 124.1(4) . . ?
C14 C9 N3 117.4(4) . . ?
C9 C10 C11 116.6(4) . . ?
C9 C10 C15 123.7(4) . . ?
C11 C10 C15 119.6(5) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 C10 121.0(5) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 H12 119.6 . . ?
C11 C12 C13 120.8(5) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 119.3 . . ?
C12 C13 C14 121.5(5) . . ?
C14 C13 H13 119.3 . . ?
C9 C14 C18 123.6(4) . . ?
C13 C14 C9 115.9(5) . . ?
C13 C14 C18 120.5(4) . . ?
C10 C15 H15 108.1 . . ?
C10 C15 C16 110.5(4) . . ?
C10 C15 C17 111.6(4) . . ?
C16 C15 H15 108.1 . . ?
C16 C15 C17 110.4(4) . . ?
C17 C15 H15 108.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18 107.7 . . ?
C14 C18 C19 109.4(4) . . ?
C14 C18 C20 113.4(4) . . ?
C19 C18 H18 107.7 . . ?
C20 C18 H18 107.7 . . ?
C20 C18 C19 110.8(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N1 117.4(4) . . ?
C26 C21 N1 119.0(4) . . ?
C26 C21 C22 123.6(4) . . ?
C21 C22 C27 123.3(4) . . ?
C23 C22 C21 116.5(5) . . ?
C23 C22 C27 120.1(4) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 C22 121.6(5) . . ?
C24 C23 H23 119.2 . . ?
C23 C24 H24 119.9 . . ?
C23 C24 C25 120.2(4) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 119.6 . . ?
C24 C25 C26 120.9(5) . . ?
C26 C25 H25 119.6 . . ?
C21 C26 C25 117.1(5) . . ?
C21 C26 C30 122.2(4) . . ?
C25 C26 C30 120.4(5) . . ?
C22 C27 H27 107.6 . . ?
C22 C27 C28 109.5(4) . . ?
C22 C27 C29 114.0(4) . . ?
C28 C27 H27 107.6 . . ?
C29 C27 H27 107.6 . . ?
C29 C27 C28 110.2(4) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C30 H30 107.6 . . ?
C26 C30 C31 109.3(4) . . ?
C26 C30 C32 114.3(4) . . ?
C31 C30 H30 107.6 . . ?
C31 C30 C32 110.1(4) . . ?
C32 C30 H30 107.6 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C1S O1S C4S 107.1(14) . . ?
O1S C1S H1SA 109.8 . . ?
O1S C1S H1SB 109.8 . . ?
O1S C1S C2S 109.2(16) . . ?
H1SA C1S H1SB 108.3 . . ?
C2S C1S H1SA 109.8 . . ?
C2S C1S H1SB 109.8 . . ?
C1S C2S H2SA 111.8 . . ?
C1S C2S H2SB 111.8 . . ?
C1S C2S C3S 100.1(15) . . ?
H2SA C2S H2SB 109.5 . . ?
C3S C2S H2SA 111.8 . . ?
C3S C2S H2SB 111.8 . . ?
C2S C3S H3SA 111.2 . . ?
C2S C3S H3SB 111.2 . . ?
H3SA C3S H3SB 109.1 . . ?
C4S C3S C2S 102.7(14) . . ?
C4S C3S H3SA 111.2 . . ?
C4S C3S H3SB 111.2 . . ?
O1S C4S C3S 106.4(14) . . ?
O1S C4S H4SA 110.4 . . ?
O1S C4S H4SB 110.4 . . ?
C3S C4S H4SA 110.4 . . ?
C3S C4S H4SB 110.4 . . ?
H4SA C4S H4SB 108.6 . . ?
_shelx_res_file
;
jr204.res created by SHELXL-2014/7
TITL JR204.res in Pccn
CELL 0.71073 17.2279 17.4336 20.9343 90 90 90
ZERR 4 0.0005 0.0005 0.0006 0 0 0
LATT 1
SYMM 0.5-X,0.5-Y,+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,-Y,0.5-Z
SFAC C H Co I N O
UNIT 272 344 4 8 24 4
SADI O1S C4S O1S C1S
SADI C3S C4S C3S C2S C1S C2S
RIGU 0.002 0.004 O1S > C4S
L.S. 20
PLAN 5
SIZE 0.05 0.03 0.015
TEMP -173.15
BOND $H
LIST 4
fmap 2
acta
TWIN -0.012 -0.988 0 -1.012 0.012 0 0 0 -1 2
OMIT 1 0 4
REM
REM
REM
WGHT 0.035000 32.371197
BASF 0.08217
FVAR 0.16139
I1 4 0.346952 0.822589 0.091013 11.00000 0.03392 0.02366 =
0.02243 0.00322 0.00898 0.00031
CO1 3 0.250000 0.750000 0.165211 10.50000 0.02042 0.01624 =
0.01110 0.00000 0.00000 0.00240
N1 5 0.363400 0.617254 0.203743 11.00000 0.02403 0.01840 =
0.01170 0.00015 -0.00111 -0.00084
N2 5 0.418000 0.593682 0.245433 11.00000 0.02185 0.01983 =
0.01357 -0.00111 -0.00339 0.00364
N3 5 0.415164 0.648033 0.290043 11.00000 0.01862 0.01947 =
0.01313 -0.00125 -0.00134 0.00086
C1 1 0.326252 0.683652 0.219405 11.00000 0.02158 0.01230 =
0.01362 -0.00314 0.00466 -0.00540
C2 1 0.360214 0.702202 0.277464 11.00000 0.02353 0.01661 =
0.01333 0.00418 0.00272 0.00121
C3 1 0.348840 0.768113 0.320775 11.00000 0.01602 0.02403 =
0.01529 -0.00128 -0.00209 0.00293
C4 1 0.346293 0.841743 0.295500 11.00000 0.02097 0.02553 =
0.01546 -0.00131 -0.00407 0.00263
AFIX 43
H4 2 0.350997 0.849090 0.250701 11.00000 -1.20000
AFIX 0
C5 1 0.336910 0.904576 0.335396 11.00000 0.03280 0.02066 =
0.02811 -0.00206 -0.01148 0.00166
AFIX 43
H5 2 0.335913 0.954874 0.317958 11.00000 -1.20000
AFIX 0
C6 1 0.328947 0.893970 0.401035 11.00000 0.02876 0.02619 =
0.02710 -0.01433 -0.00504 0.00325
AFIX 43
H6 2 0.322020 0.937013 0.428274 11.00000 -1.20000
AFIX 0
C7 1 0.331112 0.821034 0.426505 11.00000 0.02330 0.03340 =
0.01587 -0.00665 -0.00190 0.00625
AFIX 43
H7 2 0.325785 0.813943 0.471285 11.00000 -1.20000
AFIX 0
C8 1 0.341102 0.757666 0.386669 11.00000 0.02147 0.02063 =
0.01845 -0.00154 -0.00423 0.00389
AFIX 43
H8 2 0.342646 0.707476 0.404298 11.00000 -1.20000
AFIX 0
C9 1 0.468779 0.646015 0.343912 11.00000 0.02203 0.02110 =
0.01459 -0.00275 -0.00419 0.00652
C10 1 0.526317 0.702279 0.347467 11.00000 0.02428 0.01946 =
0.02015 -0.00144 -0.00042 0.00461
C11 1 0.571951 0.702821 0.402638 11.00000 0.03119 0.02537 =
0.02491 -0.00427 -0.00973 -0.00252
AFIX 43
H11 2 0.612521 0.739408 0.406677 11.00000 -1.20000
AFIX 0
C12 1 0.559069 0.651220 0.451197 11.00000 0.03682 0.02862 =
0.02478 -0.00120 -0.01324 0.00530
AFIX 43
H12 2 0.590119 0.653345 0.488657 11.00000 -1.20000
AFIX 0
C13 1 0.501742 0.596529 0.446196 11.00000 0.03582 0.02748 =
0.01884 0.00218 -0.00970 0.00558
AFIX 43
H13 2 0.493980 0.561519 0.480379 11.00000 -1.20000
AFIX 0
C14 1 0.454671 0.591342 0.391934 11.00000 0.02770 0.01980 =
0.01444 -0.00102 -0.00239 0.00513
C15 1 0.541807 0.760482 0.295013 11.00000 0.02583 0.02620 =
0.02363 0.00094 -0.00088 -0.00500
AFIX 13
H15 2 0.497894 0.758021 0.263842 11.00000 -1.20000
AFIX 0
C16 1 0.616874 0.740703 0.259290 11.00000 0.03741 0.03990 =
0.03313 -0.00338 0.00590 -0.00396
AFIX 137
H16A 2 0.660452 0.740541 0.289379 11.00000 -1.50000
H16B 2 0.626267 0.779047 0.225942 11.00000 -1.50000
H16C 2 0.611886 0.689879 0.239715 11.00000 -1.50000
AFIX 0
C17 1 0.545764 0.842392 0.321588 11.00000 0.03064 0.03040 =
0.03371 0.00281 -0.00136 -0.00537
AFIX 137
H17A 2 0.498636 0.853231 0.346200 11.00000 -1.50000
H17B 2 0.549927 0.878901 0.286157 11.00000 -1.50000
H17C 2 0.591257 0.847372 0.349384 11.00000 -1.50000
AFIX 0
C18 1 0.394456 0.528680 0.386295 11.00000 0.02717 0.02383 =
0.01556 0.00304 -0.00429 0.00150
AFIX 13
H18 2 0.356977 0.544159 0.352172 11.00000 -1.20000
AFIX 0
C19 1 0.433853 0.454184 0.364724 11.00000 0.03318 0.02687 =
0.02340 0.00033 -0.00283 -0.00202
AFIX 137
H19A 2 0.458935 0.462327 0.323258 11.00000 -1.50000
H19B 2 0.394842 0.413541 0.360825 11.00000 -1.50000
H19C 2 0.472962 0.439073 0.396303 11.00000 -1.50000
AFIX 0
C20 1 0.348101 0.515834 0.447903 11.00000 0.03237 0.03152 =
0.02052 0.00365 0.00112 0.00513
AFIX 137
H20A 2 0.382211 0.494069 0.480689 11.00000 -1.50000
H20B 2 0.305229 0.480303 0.439471 11.00000 -1.50000
H20C 2 0.327238 0.564922 0.462923 11.00000 -1.50000
AFIX 0
C21 1 0.354985 0.569545 0.146982 11.00000 0.02357 0.01469 =
0.01451 -0.00321 0.00029 0.00413
C22 1 0.410913 0.577719 0.098811 11.00000 0.02388 0.01739 =
0.01567 0.00328 -0.00023 0.00507
C23 1 0.402315 0.530880 0.045279 11.00000 0.02901 0.02330 =
0.01717 -0.00116 -0.00009 0.00938
AFIX 43
H23 2 0.438891 0.534673 0.011466 11.00000 -1.20000
AFIX 0
C24 1 0.342419 0.479518 0.040239 11.00000 0.03817 0.02292 =
0.01342 -0.00167 -0.00385 0.00929
AFIX 43
H24 2 0.337741 0.448564 0.003090 11.00000 -1.20000
AFIX 0
C25 1 0.288483 0.472539 0.089274 11.00000 0.03312 0.01570 =
0.01926 -0.00103 -0.00355 0.00215
AFIX 43
H25 2 0.247285 0.436624 0.085357 11.00000 -1.20000
AFIX 0
C26 1 0.294035 0.517474 0.144038 11.00000 0.02538 0.01651 =
0.01988 -0.00202 -0.00174 0.00672
C27 1 0.481491 0.629888 0.104895 11.00000 0.02154 0.02356 =
0.01946 -0.00248 0.00401 0.00047
AFIX 13
H27 2 0.468989 0.670039 0.137421 11.00000 -1.20000
AFIX 0
C28 1 0.550769 0.583382 0.130101 11.00000 0.02318 0.04376 =
0.02098 -0.00015 0.00056 0.00437
AFIX 137
H28A 2 0.537755 0.561623 0.171916 11.00000 -1.50000
H28B 2 0.596044 0.617034 0.134319 11.00000 -1.50000
H28C 2 0.562698 0.541821 0.100148 11.00000 -1.50000
AFIX 0
C29 1 0.503669 0.671161 0.042701 11.00000 0.03137 0.03607 =
0.01949 0.00380 0.00478 -0.00067
AFIX 137
H29A 2 0.522153 0.633521 0.011435 11.00000 -1.50000
H29B 2 0.544880 0.708469 0.051417 11.00000 -1.50000
H29C 2 0.458126 0.697827 0.025568 11.00000 -1.50000
AFIX 0
C30 1 0.239117 0.504432 0.199952 11.00000 0.02692 0.01614 =
0.02326 0.00095 -0.00082 0.00018
AFIX 13
H30 2 0.235455 0.553651 0.224297 11.00000 -1.20000
AFIX 0
C31 1 0.273926 0.443868 0.244822 11.00000 0.03352 0.02667 =
0.02196 0.00147 0.00105 0.00251
AFIX 137
H31A 2 0.275658 0.394209 0.222931 11.00000 -1.50000
H31B 2 0.241699 0.439567 0.283231 11.00000 -1.50000
H31C 2 0.326643 0.459166 0.256948 11.00000 -1.50000
AFIX 0
C32 1 0.156135 0.481174 0.180329 11.00000 0.02931 0.02843 =
0.03321 0.00351 0.00090 -0.00132
AFIX 137
H32A 2 0.135780 0.518369 0.149484 11.00000 -1.50000
H32B 2 0.122716 0.480286 0.218204 11.00000 -1.50000
H32C 2 0.157160 0.430082 0.160824 11.00000 -1.50000
AFIX 0
PART -1
O1S 6 0.253156 0.335650 0.445597 10.50000 0.08674 0.03050 =
0.04675 0.00527 0.02368 0.00068
C1S 1 0.268143 0.286234 0.392153 10.50000 0.07653 0.03838 =
0.04284 0.00190 0.01433 0.01119
AFIX 23
H1SA 2 0.324334 0.286208 0.382251 10.50000 -1.20000
H1SB 2 0.239830 0.305070 0.354107 10.50000 -1.20000
AFIX 0
C2S 1 0.242027 0.206364 0.408136 10.50000 0.07800 0.04086 =
0.04359 0.00673 -0.00115 0.00593
AFIX 23
H2SA 2 0.274631 0.167147 0.386926 10.50000 -1.20000
H2SB 2 0.186915 0.197978 0.396707 10.50000 -1.20000
AFIX 0
C3S 1 0.254065 0.206793 0.480319 10.50000 0.04300 0.03720 =
0.04343 0.00784 0.00322 0.00344
AFIX 23
H3SA 2 0.220435 0.168458 0.501562 10.50000 -1.20000
H3SB 2 0.308897 0.196307 0.491455 10.50000 -1.20000
AFIX 0
C4S 1 0.231211 0.287196 0.498493 10.50000 0.04342 0.03637 =
0.04308 0.00967 0.00771 0.00307
AFIX 23
H4SA 2 0.174578 0.290298 0.506080 10.50000 -1.20000
H4SB 2 0.258541 0.303237 0.537890 10.50000 -1.20000
AFIX 0
HKLF 4
REM JR204.res in Pccn
REM R1 = 0.0407 for 4809 Fo > 4sig(Fo) and 0.0609 for all 5958 data
REM 384 parameters refined using 34 restraints
END
WGHT 0.0338 32.6866
REM Highest difference peak 1.126, deepest hole -0.721, 1-sigma level 0.091
Q1 1 0.3045 0.8598 0.0915 11.00000 0.05 1.13
Q2 1 0.6223 0.6614 0.5093 11.00000 0.05 1.05
Q3 1 0.3188 0.4074 -0.0097 11.00000 0.05 0.83
Q4 1 0.2892 0.7979 0.0915 11.00000 0.05 0.63
Q5 1 0.3837 0.8730 0.0919 11.00000 0.05 0.60
;
_shelx_res_checksum 99097
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9178(7)
2 0.0822(7)
_chemical_properties_physical Moisture-sensitive