# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# 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.
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data_new4_ct
_database_code_depnum_ccdc_archive 'CCDC 1554856'
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_audit_creation_date 2017-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety '2(C44 H48 Mg N6), 3(C7 H8)'
_chemical_formula_sum 'C109 H120 Mg2 N12'
_chemical_formula_weight 1646.78
_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'
Mg Mg 0.0486 0.0363 '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/c 1'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 18.885(4)
_cell_length_b 12.5765(19)
_cell_length_c 21.644(4)
_cell_angle_alpha 90
_cell_angle_beta 115.462(4)
_cell_angle_gamma 90
_cell_volume 4641.3(14)
_cell_formula_units_Z 2
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 11469
_cell_measurement_theta_min 1.1942
_cell_measurement_theta_max 28.3637
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.082
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7809
_exptl_absorpt_process_details 'Blessing, 1995'
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.178
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 1764
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.15
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.1068
_diffrn_reflns_av_unetI/netI 0.1664
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 37826
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.640
_diffrn_reflns_theta_min 1.926
_diffrn_ambient_temperature 100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Sealed Tube'
_diffrn_radiation_monochromator 'Graphite Monochromator'
_diffrn_radiation_detector CCD
_diffrn_measurement_device
;
Mercury2 (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measurement_method dtprofit.ref
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5486
_reflns_number_total 11395
_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 ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.605
_refine_diff_density_min -0.317
_refine_diff_density_rms 0.060
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.010
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 546
_refine_ls_number_reflns 11395
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1845
_refine_ls_R_factor_gt 0.0864
_refine_ls_restrained_S_all 1.010
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0678P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1784
_refine_ls_wR_factor_ref 0.2189
_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. Others
Fixed Sof: C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5) C58(0.5) H58(0.5)
C57(0.5) H57(0.5) C56(0.5) H56(0.5) C55(0.5) H55(0.5) C54(0.5) H54(0.5)
3.a Free rotating group:
C52(C53,C58,C57,C56,C55,C54)
3.b Ternary CH refined with riding coordinates:
C17(H17), C20(H20), C39(H39), C42(H42)
3.c Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C10(H10), C13(H13), C14(H14),
C15(H15), C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C32(H32),
C35(H35), C36(H36), C37(H37), C46(H46), C47(H47), C48(H48), C49(H49),
C50(H50), C58(H58), C57(H57), C56(H56), C55(H55), C54(H54)
3.d Idealised Me refined as rotating group:
C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
H22C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,
H44B,H44C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_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
Mg1 Mg 0.65004(6) 0.17661(7) 0.37095(5) 0.0271(3) Uani 1 1 d . . . . .
N1 N 0.65724(15) 0.05604(18) 0.30374(13) 0.0282(6) Uani 1 1 d . . . . .
C1 C 0.6862(2) -0.0427(2) 0.30317(18) 0.0343(8) Uani 1 1 d . . . . .
H1 H 0.7230 -0.0780 0.3428 0.041 Uiso 1 1 calc R . . . .
N2 N 0.58943(15) 0.24490(18) 0.27324(13) 0.0253(6) Uani 1 1 d . . . . .
C2 C 0.6561(2) -0.0854(2) 0.23859(19) 0.0363(8) Uani 1 1 d . . . . .
H2 H 0.6680 -0.1531 0.2261 0.044 Uiso 1 1 calc R . . . .
N3 N 0.63539(15) 0.36615(18) 0.38541(13) 0.0266(6) Uani 1 1 d . . . . .
C3 C 0.6045(2) -0.0100(2) 0.19481(17) 0.0334(8) Uani 1 1 d . . . . .
H3 H 0.5739 -0.0162 0.1468 0.040 Uiso 1 1 calc R . . . .
N4 N 0.54161(16) 0.13310(18) 0.37305(14) 0.0294(6) Uani 1 1 d . . . . .
C4 C 0.60717(19) 0.0761(2) 0.23616(16) 0.0267(7) Uani 1 1 d . . . . .
N5 N 0.68373(15) 0.07125(18) 0.45551(13) 0.0264(6) Uani 1 1 d . . . . .
C5 C 0.56661(19) 0.1777(2) 0.22041(16) 0.0264(7) Uani 1 1 d . . . . .
N6 N 0.78868(15) 0.18912(18) 0.43508(13) 0.0253(6) Uani 1 1 d . . . . .
C6 C 0.5069(2) 0.2066(2) 0.15679(17) 0.0315(8) Uani 1 1 d . . . . .
H6 H 0.4912 0.1594 0.1190 0.038 Uiso 1 1 calc R . . . .
C7 C 0.4712(2) 0.3039(2) 0.14975(17) 0.0342(8) Uani 1 1 d . . . . .
H7 H 0.4304 0.3239 0.1069 0.041 Uiso 1 1 calc R . . . .
C8 C 0.49484(19) 0.3734(2) 0.20525(17) 0.0301(8) Uani 1 1 d . . . . .
H8 H 0.4711 0.4412 0.2011 0.036 Uiso 1 1 calc R . . . .
C9 C 0.55391(18) 0.3399(2) 0.26634(16) 0.0262(7) Uani 1 1 d . . . . .
C10 C 0.58362(19) 0.4038(2) 0.32857(16) 0.0262(7) Uani 1 1 d . . . . .
H10 H 0.5646 0.4740 0.3272 0.031 Uiso 1 1 calc R . . . .
C11 C 0.66251(19) 0.4411(2) 0.44182(16) 0.0267(7) Uani 1 1 d . . . . .
C12 C 0.7008(2) 0.5361(2) 0.43781(17) 0.0300(8) Uani 1 1 d . . . . .
C13 C 0.7181(2) 0.6086(2) 0.49101(17) 0.0352(8) Uani 1 1 d . . . . .
H13 H 0.7418 0.6745 0.4892 0.042 Uiso 1 1 calc R . . . .
C14 C 0.7020(2) 0.5879(3) 0.54605(18) 0.0417(9) Uani 1 1 d . . . . .
H14 H 0.7127 0.6403 0.5806 0.050 Uiso 1 1 calc R . . . .
C15 C 0.6704(2) 0.4916(2) 0.55130(18) 0.0369(8) Uani 1 1 d . . . . .
H15 H 0.6619 0.4767 0.5906 0.044 Uiso 1 1 calc R . . . .
C16 C 0.6507(2) 0.4158(2) 0.49985(17) 0.0301(8) Uani 1 1 d . . . . .
C17 C 0.6129(2) 0.3111(2) 0.50483(17) 0.0315(8) Uani 1 1 d . . . . .
H17 H 0.6192 0.2603 0.4720 0.038 Uiso 1 1 calc R . . . .
C18 C 0.5250(2) 0.3247(3) 0.48312(19) 0.0423(9) Uani 1 1 d . . . . .
H18A H 0.5167 0.3763 0.5133 0.063 Uiso 1 1 calc GR . . . .
H18B H 0.5021 0.2561 0.4863 0.063 Uiso 1 1 calc GR . . . .
H18C H 0.4998 0.3504 0.4358 0.063 Uiso 1 1 calc GR . . . .
C19 C 0.6534(2) 0.2616(3) 0.57636(18) 0.0395(9) Uani 1 1 d . . . . .
H19A H 0.7096 0.2539 0.5890 0.059 Uiso 1 1 calc GR . . . .
H19B H 0.6306 0.1916 0.5762 0.059 Uiso 1 1 calc GR . . . .
H19C H 0.6459 0.3078 0.6095 0.059 Uiso 1 1 calc GR . . . .
C20 C 0.7264(2) 0.5592(2) 0.38187(17) 0.0307(8) Uani 1 1 d . . . . .
H20 H 0.7111 0.4969 0.3501 0.037 Uiso 1 1 calc R . . . .
C21 C 0.8158(2) 0.5706(3) 0.4117(2) 0.0434(9) Uani 1 1 d . . . . .
H21A H 0.8325 0.6308 0.4436 0.065 Uiso 1 1 calc GR . . . .
H21B H 0.8313 0.5832 0.3746 0.065 Uiso 1 1 calc GR . . . .
H21C H 0.8406 0.5053 0.4361 0.065 Uiso 1 1 calc GR . . . .
C22 C 0.6864(2) 0.6569(3) 0.3403(2) 0.0493(10) Uani 1 1 d . . . . .
H22A H 0.6295 0.6465 0.3194 0.074 Uiso 1 1 calc GR . . . .
H22B H 0.7041 0.6679 0.3043 0.074 Uiso 1 1 calc GR . . . .
H22C H 0.6999 0.7192 0.3703 0.074 Uiso 1 1 calc GR . . . .
C23 C 0.4641(2) 0.1478(2) 0.33659(17) 0.0329(8) Uani 1 1 d . . . . .
H23 H 0.4418 0.1986 0.3009 0.040 Uiso 1 1 calc R . . . .
C24 C 0.4206(2) 0.0798(2) 0.35732(18) 0.0335(8) Uani 1 1 d . . . . .
H24 H 0.3650 0.0753 0.3387 0.040 Uiso 1 1 calc R . . . .
C25 C 0.4743(2) 0.0194(2) 0.41080(17) 0.0332(8) Uani 1 1 d . . . . .
H25 H 0.4626 -0.0341 0.4360 0.040 Uiso 1 1 calc R . . . .
C26 C 0.54849(19) 0.0528(2) 0.42000(16) 0.0270(7) Uani 1 1 d . . . . .
C27 C 0.62637(19) 0.0180(2) 0.46367(16) 0.0271(7) Uani 1 1 d . . . . .
C28 C 0.6463(2) -0.0659(2) 0.51172(16) 0.0289(7) Uani 1 1 d . . . . .
H28 H 0.6066 -0.1034 0.5186 0.035 Uiso 1 1 calc R . . . .
C29 C 0.7238(2) -0.0923(2) 0.54820(17) 0.0322(8) Uani 1 1 d . . . . .
H29 H 0.7378 -0.1478 0.5811 0.039 Uiso 1 1 calc R . . . .
C30 C 0.7820(2) -0.0388(2) 0.53767(16) 0.0308(8) Uani 1 1 d . . . . .
H30 H 0.8356 -0.0580 0.5617 0.037 Uiso 1 1 calc R . . . .
C31 C 0.75869(19) 0.0436(2) 0.49077(16) 0.0264(7) Uani 1 1 d . . . . .
C32 C 0.81317(19) 0.1108(2) 0.47683(16) 0.0281(7) Uani 1 1 d . . . . .
H32 H 0.8678 0.0962 0.4991 0.034 Uiso 1 1 calc R . . . .
C33 C 0.85038(19) 0.2586(2) 0.43646(17) 0.0289(7) Uani 1 1 d . . . . .
C34 C 0.8558(2) 0.2798(2) 0.37483(17) 0.0350(8) Uani 1 1 d . . . . .
C35 C 0.9212(2) 0.3372(2) 0.37964(18) 0.0354(8) Uani 1 1 d . . . . .
H35 H 0.9276 0.3513 0.3392 0.043 Uiso 1 1 calc R . . . .
C36 C 0.9769(2) 0.3741(2) 0.44171(19) 0.0370(9) Uani 1 1 d . . . . .
H36 H 1.0222 0.4098 0.4439 0.044 Uiso 1 1 calc R . . . .
C37 C 0.9666(2) 0.3591(2) 0.50028(18) 0.0354(8) Uani 1 1 d . . . . .
H37 H 1.0043 0.3872 0.5423 0.042 Uiso 1 1 calc R . . . .
C38 C 0.90214(19) 0.3034(2) 0.49932(17) 0.0301(7) Uani 1 1 d . . . . .
C39 C 0.8903(2) 0.2973(2) 0.56445(17) 0.0355(8) Uani 1 1 d . . . . .
H39 H 0.8390 0.2609 0.5529 0.043 Uiso 1 1 calc R . . . .
C40 C 0.8853(2) 0.4090(2) 0.59129(19) 0.0413(9) Uani 1 1 d . . . . .
H40A H 0.9359 0.4451 0.6056 0.062 Uiso 1 1 calc GR . . . .
H40B H 0.8724 0.4029 0.6304 0.062 Uiso 1 1 calc GR . . . .
H40C H 0.8445 0.4502 0.5549 0.062 Uiso 1 1 calc GR . . . .
C41 C 0.9539(2) 0.2337(3) 0.62143(19) 0.0465(10) Uani 1 1 d . . . . .
H41A H 0.9541 0.1606 0.6060 0.070 Uiso 1 1 calc GR . . . .
H41B H 0.9433 0.2334 0.6620 0.070 Uiso 1 1 calc GR . . . .
H41C H 1.0051 0.2665 0.6330 0.070 Uiso 1 1 calc GR . . . .
C42 C 0.7949(2) 0.2431(3) 0.30573(18) 0.0392(9) Uani 1 1 d . . . . .
H42 H 0.7518 0.2078 0.3134 0.047 Uiso 1 1 calc R . . . .
C43 C 0.8259(3) 0.1635(3) 0.2725(2) 0.0883(19) Uani 1 1 d . . . . .
H43A H 0.8658 0.1970 0.2613 0.132 Uiso 1 1 calc GR . . . .
H43B H 0.7829 0.1372 0.2305 0.132 Uiso 1 1 calc GR . . . .
H43C H 0.8494 0.1039 0.3039 0.132 Uiso 1 1 calc GR . . . .
C44 C 0.7590(3) 0.3356(3) 0.2579(2) 0.0581(12) Uani 1 1 d . . . . .
H44A H 0.7419 0.3898 0.2812 0.087 Uiso 1 1 calc GR . . . .
H44B H 0.7137 0.3108 0.2170 0.087 Uiso 1 1 calc GR . . . .
H44C H 0.7980 0.3663 0.2445 0.087 Uiso 1 1 calc GR . . . .
C45 C 0.9124(2) 0.8749(3) 0.7140(2) 0.0490(10) Uani 1 1 d . . . . .
C46 C 0.9282(2) 0.7892(3) 0.6822(2) 0.0487(10) Uani 1 1 d . . . . .
H46 H 0.9619 0.7983 0.6603 0.058 Uiso 1 1 calc R . . . .
C47 C 0.8956(3) 0.6897(3) 0.6815(2) 0.0628(13) Uani 1 1 d . . . . .
H47 H 0.9065 0.6314 0.6590 0.075 Uiso 1 1 calc R . . . .
C48 C 0.8480(3) 0.6769(4) 0.7136(2) 0.0637(13) Uani 1 1 d . . . . .
H48 H 0.8261 0.6091 0.7141 0.076 Uiso 1 1 calc R . . . .
C49 C 0.8317(3) 0.7617(4) 0.7452(2) 0.0599(12) Uani 1 1 d . . . . .
H49 H 0.7984 0.7523 0.7675 0.072 Uiso 1 1 calc R . . . .
C50 C 0.8628(3) 0.8592(3) 0.7449(2) 0.0558(11) Uani 1 1 d . . . . .
H50 H 0.8501 0.9174 0.7663 0.067 Uiso 1 1 calc R . . . .
C51 C 0.9481(3) 0.9813(3) 0.7150(2) 0.0783(15) Uani 1 1 d . . . . .
H51A H 0.9719 0.9813 0.6827 0.117 Uiso 1 1 calc GR . . . .
H51B H 0.9885 0.9961 0.7612 0.117 Uiso 1 1 calc GR . . . .
H51C H 0.9074 1.0362 0.7018 0.117 Uiso 1 1 calc GR . . . .
C52 C 1.0962(4) 0.1192(6) 0.5618(4) 0.134(7) Uiso 0.5 1 d . . P A -1
H52A H 1.1137 0.1067 0.6109 0.201 Uiso 0.5 1 calc GR . P A -1
H52B H 1.0763 0.1920 0.5506 0.201 Uiso 0.5 1 calc GR . P A -1
H52C H 1.1404 0.1093 0.5500 0.201 Uiso 0.5 1 calc GR . P A -1
C53 C 1.0319(3) 0.0417(4) 0.5217(3) 0.068(3) Uiso 0.5 1 d G . P A -1
C58 C 1.0146(4) -0.0444(5) 0.5540(3) 0.079(7) Uiso 0.5 1 d G . P A -1
H58 H 1.0430 -0.0529 0.6021 0.094 Uiso 0.5 1 calc R . P A -1
C57 C 0.9563(4) -0.1177(4) 0.5168(3) 0.068(3) Uiso 0.5 1 d G . P A -1
H57 H 0.9454 -0.1756 0.5396 0.082 Uiso 0.5 1 calc R . P A -1
C56 C 0.9140(3) -0.1061(4) 0.4461(3) 0.049(3) Uiso 0.5 1 d G . P A -1
H56 H 0.8744 -0.1560 0.4206 0.059 Uiso 0.5 1 calc R . P A -1
C55 C 0.9304(3) -0.0206(4) 0.4131(3) 0.062(2) Uiso 0.5 1 d G . P A -1
H55 H 0.9017 -0.0122 0.3651 0.075 Uiso 0.5 1 calc R . P A -1
C54 C 0.9887(3) 0.0524(4) 0.4507(3) 0.043(4) Uiso 0.5 1 d G . P A -1
H54 H 0.9994 0.1104 0.4278 0.051 Uiso 0.5 1 calc R . P 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
Mg1 0.0268(6) 0.0281(5) 0.0239(6) 0.0014(4) 0.0085(5) 0.0000(4)
N1 0.0289(16) 0.0286(14) 0.0246(15) 0.0004(11) 0.0093(13) -0.0014(11)
C1 0.034(2) 0.0255(17) 0.039(2) 0.0018(14) 0.0112(17) 0.0066(14)
N2 0.0256(15) 0.0271(13) 0.0227(15) -0.0001(11) 0.0098(13) 0.0007(11)
C2 0.038(2) 0.0303(17) 0.044(2) -0.0040(16) 0.0211(19) 0.0000(15)
N3 0.0280(16) 0.0286(13) 0.0236(15) -0.0003(11) 0.0114(13) -0.0031(11)
C3 0.037(2) 0.0388(19) 0.0246(19) -0.0056(14) 0.0137(17) -0.0074(15)
N4 0.0279(17) 0.0313(14) 0.0262(16) 0.0015(11) 0.0089(13) 0.0011(11)
C4 0.032(2) 0.0255(16) 0.0252(18) 0.0001(13) 0.0145(16) -0.0020(13)
N5 0.0247(16) 0.0281(13) 0.0240(15) -0.0019(11) 0.0082(13) -0.0020(11)
C5 0.0285(19) 0.0290(17) 0.0226(17) -0.0014(13) 0.0118(15) -0.0058(13)
N6 0.0245(15) 0.0271(13) 0.0221(14) -0.0009(11) 0.0078(12) -0.0012(11)
C6 0.034(2) 0.0342(18) 0.0229(18) -0.0005(13) 0.0093(16) -0.0030(14)
C7 0.031(2) 0.042(2) 0.0215(18) 0.0061(14) 0.0044(16) -0.0004(15)
C8 0.029(2) 0.0311(17) 0.0277(19) 0.0034(14) 0.0097(16) 0.0011(14)
C9 0.0253(18) 0.0292(16) 0.0239(18) 0.0013(13) 0.0104(15) 0.0001(13)
C10 0.0281(19) 0.0263(16) 0.0238(18) 0.0015(13) 0.0109(16) 0.0002(13)
C11 0.0265(19) 0.0286(16) 0.0209(17) -0.0023(12) 0.0063(15) 0.0031(13)
C12 0.032(2) 0.0273(16) 0.0288(19) 0.0013(13) 0.0114(16) 0.0005(13)
C13 0.043(2) 0.0320(18) 0.030(2) -0.0029(14) 0.0156(18) -0.0049(15)
C14 0.057(3) 0.037(2) 0.029(2) -0.0136(15) 0.017(2) -0.0061(17)
C15 0.048(2) 0.0373(19) 0.0283(19) -0.0018(15) 0.0190(18) -0.0059(16)
C16 0.036(2) 0.0276(17) 0.0274(19) 0.0009(13) 0.0141(17) 0.0031(13)
C17 0.038(2) 0.0321(17) 0.0245(18) 0.0001(13) 0.0129(17) -0.0009(14)
C18 0.039(2) 0.049(2) 0.035(2) 0.0045(16) 0.0121(19) -0.0057(17)
C19 0.042(2) 0.042(2) 0.031(2) 0.0035(15) 0.0122(18) -0.0027(16)
C20 0.035(2) 0.0285(17) 0.0267(19) 0.0016(13) 0.0117(17) -0.0020(13)
C21 0.039(2) 0.049(2) 0.043(2) 0.0085(17) 0.019(2) 0.0040(17)
C22 0.052(3) 0.052(2) 0.045(2) 0.0207(18) 0.022(2) 0.0107(18)
C23 0.031(2) 0.0383(18) 0.0256(19) 0.0008(14) 0.0087(17) 0.0029(14)
C24 0.0216(19) 0.0455(19) 0.033(2) -0.0008(15) 0.0115(17) -0.0023(14)
C25 0.034(2) 0.0312(17) 0.032(2) 0.0000(14) 0.0118(17) -0.0045(14)
C26 0.0282(19) 0.0283(16) 0.0238(18) -0.0039(13) 0.0104(16) -0.0024(13)
C27 0.0306(19) 0.0285(16) 0.0234(18) -0.0041(13) 0.0127(16) -0.0033(13)
C28 0.033(2) 0.0284(17) 0.0269(19) 0.0004(13) 0.0143(17) -0.0058(13)
C29 0.040(2) 0.0298(17) 0.0240(18) 0.0035(13) 0.0112(17) -0.0013(14)
C30 0.032(2) 0.0291(17) 0.0263(19) 0.0011(13) 0.0074(16) 0.0029(14)
C31 0.0253(19) 0.0282(16) 0.0235(17) 0.0002(13) 0.0083(15) -0.0009(13)
C32 0.0251(19) 0.0338(17) 0.0241(18) 0.0013(14) 0.0093(16) 0.0020(13)
C33 0.0285(19) 0.0284(16) 0.0287(19) 0.0010(13) 0.0113(16) -0.0029(13)
C34 0.040(2) 0.0348(18) 0.029(2) 0.0008(14) 0.0136(18) -0.0041(15)
C35 0.042(2) 0.0376(18) 0.033(2) -0.0013(15) 0.0220(18) -0.0053(15)
C36 0.031(2) 0.0348(18) 0.048(2) -0.0045(16) 0.0191(19) -0.0083(14)
C37 0.032(2) 0.0348(18) 0.032(2) -0.0023(14) 0.0071(17) -0.0041(14)
C38 0.0281(19) 0.0310(17) 0.0280(19) -0.0018(13) 0.0089(16) -0.0025(13)
C39 0.035(2) 0.0384(19) 0.029(2) -0.0019(14) 0.0093(17) -0.0036(15)
C40 0.048(2) 0.043(2) 0.039(2) -0.0047(16) 0.024(2) -0.0018(16)
C41 0.054(3) 0.048(2) 0.029(2) 0.0028(16) 0.010(2) 0.0029(18)
C42 0.046(2) 0.044(2) 0.028(2) -0.0023(15) 0.0164(19) -0.0165(16)
C43 0.098(4) 0.064(3) 0.053(3) -0.022(2) -0.015(3) 0.037(3)
C44 0.054(3) 0.056(2) 0.042(3) -0.0131(19) 0.000(2) 0.010(2)
C45 0.051(3) 0.052(2) 0.032(2) 0.0029(17) 0.007(2) -0.0009(19)
C46 0.046(3) 0.063(3) 0.036(2) -0.0017(19) 0.018(2) 0.0069(19)
C47 0.074(4) 0.056(3) 0.046(3) -0.005(2) 0.014(3) 0.011(2)
C48 0.066(3) 0.067(3) 0.046(3) 0.007(2) 0.014(3) -0.016(2)
C49 0.043(3) 0.085(3) 0.055(3) 0.002(2) 0.023(2) -0.001(2)
C50 0.054(3) 0.073(3) 0.042(3) 0.001(2) 0.022(2) 0.011(2)
C51 0.103(4) 0.065(3) 0.052(3) 0.000(2) 0.019(3) -0.021(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
Mg1 N1 2.146(3) . ?
Mg1 N2 2.107(3) . ?
Mg1 N3 2.435(3) . ?
Mg1 N4 2.139(3) . ?
Mg1 N5 2.123(3) . ?
Mg1 N6 2.384(3) . ?
N1 C1 1.359(4) . ?
N1 C4 1.381(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.372(5) . ?
N2 C5 1.336(4) . ?
N2 C9 1.347(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.397(5) . ?
N3 C10 1.288(4) . ?
N3 C11 1.451(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.392(4) . ?
N4 C23 1.344(4) . ?
N4 C26 1.398(4) . ?
C4 C5 1.453(4) . ?
N5 C27 1.348(4) . ?
N5 C31 1.334(4) . ?
C5 C6 1.402(4) . ?
N6 C32 1.281(4) . ?
N6 C33 1.446(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.373(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.395(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.379(4) . ?
C9 C10 1.458(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.418(4) . ?
C11 C16 1.403(4) . ?
C12 C13 1.393(4) . ?
C12 C20 1.512(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.375(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.377(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.390(4) . ?
C16 C17 1.524(4) . ?
C17 H17 1.0000 . ?
C17 C18 1.528(5) . ?
C17 C19 1.533(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20 1.0000 . ?
C20 C21 1.533(5) . ?
C20 C22 1.518(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 0.9500 . ?
C23 C24 1.387(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.391(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.393(4) . ?
C26 C27 1.433(4) . ?
C27 C28 1.414(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.373(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.388(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.383(4) . ?
C31 C32 1.460(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.406(5) . ?
C33 C38 1.407(5) . ?
C34 C35 1.395(5) . ?
C34 C42 1.515(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.383(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.375(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.398(5) . ?
C38 C39 1.522(5) . ?
C39 H39 1.0000 . ?
C39 C40 1.538(4) . ?
C39 C41 1.526(5) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42 1.0000 . ?
C42 C43 1.492(6) . ?
C42 C44 1.510(5) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.379(5) . ?
C45 C50 1.378(6) . ?
C45 C51 1.495(5) . ?
C46 H46 0.9500 . ?
C46 C47 1.393(6) . ?
C47 H47 0.9500 . ?
C47 C48 1.361(6) . ?
C48 H48 0.9500 . ?
C48 C49 1.372(6) . ?
C49 H49 0.9500 . ?
C49 C50 1.361(6) . ?
C50 H50 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C52 C53 1.5073 . ?
C53 C58 1.4021 . ?
C53 C54 1.4020 . ?
C58 H58 0.9500 . ?
C58 C57 1.3962 . ?
C57 H57 0.9500 . ?
C57 C56 1.3964 . ?
C56 H56 0.9500 . ?
C56 C55 1.3965 . ?
C55 H55 0.9500 . ?
C55 C54 1.3966 . ?
C54 H54 0.9500 . ?
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
N1 Mg1 N3 145.35(10) . . ?
N1 Mg1 N6 93.87(10) . . ?
N2 Mg1 N1 76.88(10) . . ?
N2 Mg1 N3 71.78(9) . . ?
N2 Mg1 N4 90.78(11) . . ?
N2 Mg1 N5 162.12(11) . . ?
N2 Mg1 N6 122.97(10) . . ?
N4 Mg1 N1 100.01(10) . . ?
N4 Mg1 N3 94.87(9) . . ?
N4 Mg1 N6 145.75(11) . . ?
N5 Mg1 N1 93.47(10) . . ?
N5 Mg1 N3 120.57(10) . . ?
N5 Mg1 N4 75.93(11) . . ?
N5 Mg1 N6 72.08(10) . . ?
N6 Mg1 N3 91.01(9) . . ?
C1 N1 Mg1 142.6(2) . . ?
C1 N1 C4 104.6(3) . . ?
C4 N1 Mg1 112.00(19) . . ?
N1 C1 H1 124.0 . . ?
N1 C1 C2 112.0(3) . . ?
C2 C1 H1 124.0 . . ?
C5 N2 Mg1 115.94(19) . . ?
C5 N2 C9 120.3(3) . . ?
C9 N2 Mg1 120.2(2) . . ?
C1 C2 H2 126.6 . . ?
C1 C2 C3 106.8(3) . . ?
C3 C2 H2 126.6 . . ?
C10 N3 Mg1 108.56(19) . . ?
C10 N3 C11 114.4(2) . . ?
C11 N3 Mg1 136.53(19) . . ?
C2 C3 H3 127.2 . . ?
C4 C3 C2 105.7(3) . . ?
C4 C3 H3 127.2 . . ?
C23 N4 Mg1 139.8(2) . . ?
C23 N4 C26 105.3(3) . . ?
C26 N4 Mg1 114.2(2) . . ?
N1 C4 C3 111.0(3) . . ?
N1 C4 C5 117.5(3) . . ?
C3 C4 C5 131.6(3) . . ?
C27 N5 Mg1 117.6(2) . . ?
C31 N5 Mg1 120.5(2) . . ?
C31 N5 C27 120.7(3) . . ?
N2 C5 C4 114.3(3) . . ?
N2 C5 C6 120.3(3) . . ?
C6 C5 C4 125.4(3) . . ?
C32 N6 Mg1 109.4(2) . . ?
C32 N6 C33 114.0(3) . . ?
C33 N6 Mg1 136.51(19) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 C5 119.3(3) . . ?
C7 C6 H6 120.4 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.2(3) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 121.2 . . ?
C9 C8 C7 117.5(3) . . ?
C9 C8 H8 121.2 . . ?
N2 C9 C8 122.4(3) . . ?
N2 C9 C10 114.3(3) . . ?
C8 C9 C10 123.3(3) . . ?
N3 C10 C9 120.8(3) . . ?
N3 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 N3 120.1(3) . . ?
C16 C11 N3 118.1(3) . . ?
C16 C11 C12 121.8(3) . . ?
C11 C12 C20 123.9(3) . . ?
C13 C12 C11 116.5(3) . . ?
C13 C12 C20 119.6(3) . . ?
C12 C13 H13 119.0 . . ?
C14 C13 C12 122.1(3) . . ?
C14 C13 H13 119.0 . . ?
C13 C14 H14 119.9 . . ?
C13 C14 C15 120.2(3) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 120.9(3) . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C17 121.3(3) . . ?
C15 C16 C11 118.1(3) . . ?
C15 C16 C17 120.5(3) . . ?
C16 C17 H17 107.4 . . ?
C16 C17 C18 111.2(3) . . ?
C16 C17 C19 112.1(3) . . ?
C18 C17 H17 107.4 . . ?
C18 C17 C19 111.1(3) . . ?
C19 C17 H17 107.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C12 C20 H20 107.7 . . ?
C12 C20 C21 110.7(3) . . ?
C12 C20 C22 112.4(3) . . ?
C21 C20 H20 107.7 . . ?
C22 C20 H20 107.7 . . ?
C22 C20 C21 110.5(3) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 H23 124.1 . . ?
N4 C23 C24 111.9(3) . . ?
C24 C23 H23 124.1 . . ?
C23 C24 H24 126.7 . . ?
C23 C24 C25 106.5(3) . . ?
C25 C24 H24 126.7 . . ?
C24 C25 H25 126.8 . . ?
C24 C25 C26 106.4(3) . . ?
C26 C25 H25 126.8 . . ?
N4 C26 C27 116.6(3) . . ?
C25 C26 N4 109.9(3) . . ?
C25 C26 C27 133.3(3) . . ?
N5 C27 C26 114.6(3) . . ?
N5 C27 C28 119.5(3) . . ?
C28 C27 C26 125.9(3) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 C27 118.9(3) . . ?
C29 C28 H28 120.5 . . ?
C28 C29 H29 119.6 . . ?
C28 C29 C30 120.8(3) . . ?
C30 C29 H29 119.6 . . ?
C29 C30 H30 121.3 . . ?
C31 C30 C29 117.3(3) . . ?
C31 C30 H30 121.3 . . ?
N5 C31 C30 122.7(3) . . ?
N5 C31 C32 113.5(3) . . ?
C30 C31 C32 123.8(3) . . ?
N6 C32 C31 121.2(3) . . ?
N6 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C34 C33 N6 118.8(3) . . ?
C38 C33 N6 118.7(3) . . ?
C38 C33 C34 122.5(3) . . ?
C33 C34 C42 123.0(3) . . ?
C35 C34 C33 116.8(3) . . ?
C35 C34 C42 120.3(3) . . ?
C34 C35 H35 119.1 . . ?
C36 C35 C34 121.7(3) . . ?
C36 C35 H35 119.1 . . ?
C35 C36 H36 120.0 . . ?
C37 C36 C35 120.0(3) . . ?
C37 C36 H36 120.0 . . ?
C36 C37 H37 119.3 . . ?
C36 C37 C38 121.5(3) . . ?
C38 C37 H37 119.3 . . ?
C33 C38 C39 123.9(3) . . ?
C37 C38 C33 117.0(3) . . ?
C37 C38 C39 119.1(3) . . ?
C38 C39 H39 107.6 . . ?
C38 C39 C40 111.2(3) . . ?
C38 C39 C41 113.4(3) . . ?
C40 C39 H39 107.6 . . ?
C41 C39 H39 107.6 . . ?
C41 C39 C40 109.1(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C34 C42 H42 107.3 . . ?
C43 C42 C34 113.1(3) . . ?
C43 C42 H42 107.3 . . ?
C43 C42 C44 109.9(3) . . ?
C44 C42 C34 111.6(3) . . ?
C44 C42 H42 107.3 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 C51 120.8(4) . . ?
C50 C45 C46 117.9(4) . . ?
C50 C45 C51 121.2(4) . . ?
C45 C46 H46 119.4 . . ?
C45 C46 C47 121.2(4) . . ?
C47 C46 H46 119.4 . . ?
C46 C47 H47 120.4 . . ?
C48 C47 C46 119.1(4) . . ?
C48 C47 H47 120.4 . . ?
C47 C48 H48 119.9 . . ?
C47 C48 C49 120.2(4) . . ?
C49 C48 H48 119.9 . . ?
C48 C49 H49 119.8 . . ?
C50 C49 C48 120.5(4) . . ?
C50 C49 H49 119.8 . . ?
C45 C50 H50 119.4 . . ?
C49 C50 C45 121.1(4) . . ?
C49 C50 H50 119.4 . . ?
C45 C51 H51A 109.5 . . ?
C45 C51 H51B 109.5 . . ?
C45 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
C58 C53 C52 121.0 . . ?
C54 C53 C52 120.9 . . ?
C54 C53 C58 118.1 . . ?
C53 C58 H58 119.4 . . ?
C57 C58 C53 121.1 . . ?
C57 C58 H58 119.4 . . ?
C58 C57 H57 119.9 . . ?
C58 C57 C56 120.1 . . ?
C56 C57 H57 119.9 . . ?
C57 C56 H56 120.3 . . ?
C57 C56 C55 119.4 . . ?
C55 C56 H56 120.3 . . ?
C56 C55 H55 119.9 . . ?
C56 C55 C54 120.1 . . ?
C54 C55 H55 119.9 . . ?
C53 C54 H54 119.5 . . ?
C55 C54 C53 121.1 . . ?
C55 C54 H54 119.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mg1 N1 C1 C2 168.0(3) . . . . ?
Mg1 N1 C4 C3 -171.5(2) . . . . ?
Mg1 N1 C4 C5 7.4(3) . . . . ?
Mg1 N2 C5 C4 -18.2(3) . . . . ?
Mg1 N2 C5 C6 160.4(2) . . . . ?
Mg1 N2 C9 C8 -159.6(2) . . . . ?
Mg1 N2 C9 C10 20.8(3) . . . . ?
Mg1 N3 C10 C9 -10.0(4) . . . . ?
Mg1 N3 C11 C12 127.7(3) . . . . ?
Mg1 N3 C11 C16 -51.4(4) . . . . ?
Mg1 N4 C23 C24 167.7(2) . . . . ?
Mg1 N4 C26 C25 -171.4(2) . . . . ?
Mg1 N4 C26 C27 5.3(3) . . . . ?
Mg1 N5 C27 C26 -9.7(3) . . . . ?
Mg1 N5 C27 C28 169.2(2) . . . . ?
Mg1 N5 C31 C30 -167.8(2) . . . . ?
Mg1 N5 C31 C32 14.4(3) . . . . ?
Mg1 N6 C32 C31 -13.0(3) . . . . ?
Mg1 N6 C33 C34 -51.0(4) . . . . ?
Mg1 N6 C33 C38 128.2(3) . . . . ?
N1 C1 C2 C3 -0.1(4) . . . . ?
N1 C4 C5 N2 6.8(4) . . . . ?
N1 C4 C5 C6 -171.7(3) . . . . ?
C1 N1 C4 C3 1.0(4) . . . . ?
C1 N1 C4 C5 179.9(3) . . . . ?
C1 C2 C3 C4 0.7(4) . . . . ?
N2 C5 C6 C7 -1.1(5) . . . . ?
N2 C9 C10 N3 -4.8(4) . . . . ?
C2 C3 C4 N1 -1.1(4) . . . . ?
C2 C3 C4 C5 -179.8(3) . . . . ?
N3 C11 C12 C13 173.9(3) . . . . ?
N3 C11 C12 C20 -9.1(5) . . . . ?
N3 C11 C16 C15 -174.5(3) . . . . ?
N3 C11 C16 C17 1.9(4) . . . . ?
C3 C4 C5 N2 -174.6(3) . . . . ?
C3 C4 C5 C6 6.9(5) . . . . ?
N4 C23 C24 C25 0.7(4) . . . . ?
N4 C26 C27 N5 2.7(4) . . . . ?
N4 C26 C27 C28 -176.1(3) . . . . ?
C4 N1 C1 C2 -0.6(4) . . . . ?
C4 C5 C6 C7 177.3(3) . . . . ?
N5 C27 C28 C29 -1.1(4) . . . . ?
N5 C31 C32 N6 1.0(4) . . . . ?
C5 N2 C9 C8 -1.8(5) . . . . ?
C5 N2 C9 C10 178.6(3) . . . . ?
C5 C6 C7 C8 0.6(5) . . . . ?
N6 C33 C34 C35 -173.0(3) . . . . ?
N6 C33 C34 C42 6.8(5) . . . . ?
N6 C33 C38 C37 172.2(3) . . . . ?
N6 C33 C38 C39 -9.7(5) . . . . ?
C6 C7 C8 C9 -0.6(5) . . . . ?
C7 C8 C9 N2 1.2(5) . . . . ?
C7 C8 C9 C10 -179.2(3) . . . . ?
C8 C9 C10 N3 175.5(3) . . . . ?
C9 N2 C5 C4 -176.9(3) . . . . ?
C9 N2 C5 C6 1.7(4) . . . . ?
C10 N3 C11 C12 -61.4(4) . . . . ?
C10 N3 C11 C16 119.6(3) . . . . ?
C11 N3 C10 C9 176.6(3) . . . . ?
C11 C12 C13 C14 2.5(5) . . . . ?
C11 C12 C20 C21 -117.1(3) . . . . ?
C11 C12 C20 C22 118.7(3) . . . . ?
C11 C16 C17 C18 -95.8(4) . . . . ?
C11 C16 C17 C19 139.1(3) . . . . ?
C12 C11 C16 C15 6.5(5) . . . . ?
C12 C11 C16 C17 -177.2(3) . . . . ?
C12 C13 C14 C15 2.4(6) . . . . ?
C13 C12 C20 C21 59.8(4) . . . . ?
C13 C12 C20 C22 -64.4(4) . . . . ?
C13 C14 C15 C16 -3.1(6) . . . . ?
C14 C15 C16 C11 -1.3(5) . . . . ?
C14 C15 C16 C17 -177.6(3) . . . . ?
C15 C16 C17 C18 80.4(4) . . . . ?
C15 C16 C17 C19 -44.7(4) . . . . ?
C16 C11 C12 C13 -7.1(5) . . . . ?
C16 C11 C12 C20 169.9(3) . . . . ?
C20 C12 C13 C14 -174.6(3) . . . . ?
C23 N4 C26 C25 0.4(3) . . . . ?
C23 N4 C26 C27 177.2(3) . . . . ?
C23 C24 C25 C26 -0.5(4) . . . . ?
C24 C25 C26 N4 0.0(4) . . . . ?
C24 C25 C26 C27 -176.0(3) . . . . ?
C25 C26 C27 N5 178.5(3) . . . . ?
C25 C26 C27 C28 -0.3(6) . . . . ?
C26 N4 C23 C24 -0.7(3) . . . . ?
C26 C27 C28 C29 177.7(3) . . . . ?
C27 N5 C31 C30 -0.9(4) . . . . ?
C27 N5 C31 C32 -178.8(3) . . . . ?
C27 C28 C29 C30 -0.9(5) . . . . ?
C28 C29 C30 C31 1.9(5) . . . . ?
C29 C30 C31 N5 -1.0(5) . . . . ?
C29 C30 C31 C32 176.6(3) . . . . ?
C30 C31 C32 N6 -176.8(3) . . . . ?
C31 N5 C27 C26 -176.9(3) . . . . ?
C31 N5 C27 C28 2.0(4) . . . . ?
C32 N6 C33 C34 125.8(3) . . . . ?
C32 N6 C33 C38 -55.0(4) . . . . ?
C33 N6 C32 C31 169.4(3) . . . . ?
C33 C34 C35 C36 -1.8(5) . . . . ?
C33 C34 C42 C43 -114.5(4) . . . . ?
C33 C34 C42 C44 121.0(4) . . . . ?
C33 C38 C39 C40 -121.1(3) . . . . ?
C33 C38 C39 C41 115.5(4) . . . . ?
C34 C33 C38 C37 -8.6(5) . . . . ?
C34 C33 C38 C39 169.5(3) . . . . ?
C34 C35 C36 C37 -3.2(5) . . . . ?
C35 C34 C42 C43 65.2(4) . . . . ?
C35 C34 C42 C44 -59.2(5) . . . . ?
C35 C36 C37 C38 2.4(5) . . . . ?
C36 C37 C38 C33 3.3(5) . . . . ?
C36 C37 C38 C39 -174.9(3) . . . . ?
C37 C38 C39 C40 56.9(4) . . . . ?
C37 C38 C39 C41 -66.5(4) . . . . ?
C38 C33 C34 C35 7.9(5) . . . . ?
C38 C33 C34 C42 -172.4(3) . . . . ?
C42 C34 C35 C36 178.4(3) . . . . ?
C45 C46 C47 C48 -0.7(6) . . . . ?
C46 C45 C50 C49 1.4(6) . . . . ?
C46 C47 C48 C49 0.9(7) . . . . ?
C47 C48 C49 C50 0.0(7) . . . . ?
C48 C49 C50 C45 -1.2(7) . . . . ?
C50 C45 C46 C47 -0.5(6) . . . . ?
C51 C45 C46 C47 179.5(4) . . . . ?
C51 C45 C50 C49 -178.5(4) . . . . ?
C52 C53 C58 C57 -178.5 . . . . ?
C52 C53 C54 C55 178.5 . . . . ?
C53 C58 C57 C56 -0.1 . . . . ?
C58 C53 C54 C55 -0.3 . . . . ?
C58 C57 C56 C55 -0.1 . . . . ?
C57 C56 C55 C54 0.1 . . . . ?
C56 C55 C54 C53 0.1 . . . . ?
C54 C53 C58 C57 0.2 . . . . ?
_shelx_res_file
;
new4_ct.res created by SHELXL-2014/7
TITL ila2_mg rigid group refinement
CELL 0.71073 18.8854 12.5765 21.6437 90 115.462 90
ZERR 2 0.0035 0.0019 0.0038 0 0.004 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Mg N
UNIT 218 240 4 24
L.S. 20
PLAN 25
TEMP -173.15
MORE -1
BOND $H
CONF
fmap 2
acta
OMIT -8 1 6
OMIT -18 2 10
OMIT 1 2 2
REM
REM
REM
WGHT 0.067800
FVAR 1.05470
MG1 3 0.650044 0.176608 0.370955 11.00000 0.02683 0.02812 =
0.02393 0.00138 0.00851 0.00003
N1 4 0.657235 0.056035 0.303743 11.00000 0.02893 0.02862 =
0.02462 0.00038 0.00927 -0.00142
C1 1 0.686238 -0.042691 0.303175 11.00000 0.03384 0.02548 =
0.03883 0.00183 0.01117 0.00664
AFIX 43
H1 2 0.723026 -0.077954 0.342797 11.00000 -1.20000
AFIX 0
N2 4 0.589432 0.244902 0.273237 11.00000 0.02559 0.02713 =
0.02266 -0.00014 0.00979 0.00073
C2 1 0.656074 -0.085357 0.238591 11.00000 0.03807 0.03032 =
0.04421 -0.00403 0.02106 -0.00005
AFIX 43
H2 2 0.667977 -0.153100 0.226051 11.00000 -1.20000
AFIX 0
N3 4 0.635392 0.366149 0.385411 11.00000 0.02796 0.02858 =
0.02356 -0.00031 0.01138 -0.00313
C3 1 0.604477 -0.009997 0.194811 11.00000 0.03721 0.03877 =
0.02455 -0.00564 0.01370 -0.00741
AFIX 43
H3 2 0.573922 -0.016233 0.146825 11.00000 -1.20000
AFIX 0
N4 4 0.541609 0.133104 0.373047 11.00000 0.02792 0.03128 =
0.02619 0.00151 0.00891 0.00106
C4 1 0.607173 0.076134 0.236159 11.00000 0.03185 0.02552 =
0.02520 0.00012 0.01448 -0.00196
N5 4 0.683731 0.071248 0.455514 11.00000 0.02466 0.02809 =
0.02400 -0.00195 0.00825 -0.00201
C5 1 0.566612 0.177693 0.220408 11.00000 0.02852 0.02901 =
0.02256 -0.00138 0.01176 -0.00583
N6 4 0.788683 0.189119 0.435075 11.00000 0.02452 0.02713 =
0.02208 -0.00091 0.00783 -0.00116
C6 1 0.506883 0.206574 0.156786 11.00000 0.03431 0.03422 =
0.02287 -0.00054 0.00934 -0.00296
AFIX 43
H6 2 0.491236 0.159353 0.118952 11.00000 -1.20000
AFIX 0
C7 1 0.471243 0.303864 0.149752 11.00000 0.03126 0.04248 =
0.02152 0.00609 0.00437 -0.00037
AFIX 43
H7 2 0.430386 0.323903 0.106949 11.00000 -1.20000
AFIX 0
C8 1 0.494839 0.373358 0.205252 11.00000 0.02885 0.03107 =
0.02769 0.00343 0.00965 0.00114
AFIX 43
H8 2 0.471108 0.441205 0.201126 11.00000 -1.20000
AFIX 0
C9 1 0.553910 0.339888 0.266343 11.00000 0.02526 0.02915 =
0.02395 0.00132 0.01036 0.00006
C10 1 0.583620 0.403768 0.328569 11.00000 0.02814 0.02633 =
0.02376 0.00148 0.01094 0.00024
AFIX 43
H10 2 0.564556 0.474048 0.327186 11.00000 -1.20000
AFIX 0
C11 1 0.662511 0.441112 0.441820 11.00000 0.02650 0.02861 =
0.02092 -0.00230 0.00629 0.00314
C12 1 0.700790 0.536125 0.437808 11.00000 0.03218 0.02731 =
0.02878 0.00133 0.01140 0.00045
C13 1 0.718121 0.608647 0.491007 11.00000 0.04341 0.03204 =
0.03001 -0.00293 0.01563 -0.00492
AFIX 43
H13 2 0.741811 0.674494 0.489202 11.00000 -1.20000
AFIX 0
C14 1 0.702023 0.587937 0.546050 11.00000 0.05748 0.03737 =
0.02892 -0.01358 0.01730 -0.00609
AFIX 43
H14 2 0.712745 0.640282 0.580569 11.00000 -1.20000
AFIX 0
C15 1 0.670404 0.491551 0.551303 11.00000 0.04774 0.03727 =
0.02834 -0.00180 0.01896 -0.00586
AFIX 43
H15 2 0.661934 0.476684 0.590640 11.00000 -1.20000
AFIX 0
C16 1 0.650727 0.415766 0.499851 11.00000 0.03572 0.02764 =
0.02739 0.00086 0.01406 0.00310
C17 1 0.612885 0.311056 0.504835 11.00000 0.03752 0.03210 =
0.02452 0.00006 0.01288 -0.00092
AFIX 13
H17 2 0.619194 0.260283 0.471993 11.00000 -1.20000
AFIX 0
C18 1 0.524991 0.324690 0.483120 11.00000 0.03948 0.04870 =
0.03467 0.00454 0.01207 -0.00570
AFIX 137
H18A 2 0.516682 0.376276 0.513302 11.00000 -1.50000
H18B 2 0.502106 0.256148 0.486320 11.00000 -1.50000
H18C 2 0.499813 0.350389 0.435810 11.00000 -1.50000
AFIX 0
C19 1 0.653400 0.261638 0.576357 11.00000 0.04159 0.04244 =
0.03097 0.00353 0.01224 -0.00265
AFIX 137
H19A 2 0.709586 0.253887 0.589033 11.00000 -1.50000
H19B 2 0.630575 0.191606 0.576216 11.00000 -1.50000
H19C 2 0.645940 0.307826 0.609549 11.00000 -1.50000
AFIX 0
C20 1 0.726382 0.559183 0.381870 11.00000 0.03517 0.02845 =
0.02668 0.00162 0.01170 -0.00199
AFIX 13
H20 2 0.711104 0.496871 0.350084 11.00000 -1.20000
AFIX 0
C21 1 0.815774 0.570645 0.411741 11.00000 0.03933 0.04926 =
0.04298 0.00845 0.01901 0.00400
AFIX 137
H21A 2 0.832537 0.630788 0.443612 11.00000 -1.50000
H21B 2 0.831334 0.583162 0.374601 11.00000 -1.50000
H21C 2 0.840595 0.505312 0.436106 11.00000 -1.50000
AFIX 0
C22 1 0.686424 0.656871 0.340295 11.00000 0.05238 0.05230 =
0.04486 0.02068 0.02242 0.01066
AFIX 137
H22A 2 0.629462 0.646518 0.319399 11.00000 -1.50000
H22B 2 0.704094 0.667912 0.304318 11.00000 -1.50000
H22C 2 0.699920 0.719243 0.370330 11.00000 -1.50000
AFIX 0
C23 1 0.464084 0.147771 0.336595 11.00000 0.03126 0.03825 =
0.02565 0.00078 0.00875 0.00293
AFIX 43
H23 2 0.441763 0.198599 0.300926 11.00000 -1.20000
AFIX 0
C24 1 0.420591 0.079765 0.357323 11.00000 0.02155 0.04555 =
0.03303 -0.00084 0.01151 -0.00234
AFIX 43
H24 2 0.365042 0.075312 0.338663 11.00000 -1.20000
AFIX 0
C25 1 0.474277 0.019352 0.410801 11.00000 0.03396 0.03124 =
0.03197 -0.00003 0.01179 -0.00455
AFIX 43
H25 2 0.462635 -0.034123 0.436047 11.00000 -1.20000
AFIX 0
C26 1 0.548490 0.052811 0.419995 11.00000 0.02816 0.02830 =
0.02382 -0.00391 0.01043 -0.00241
C27 1 0.626368 0.018027 0.463672 11.00000 0.03061 0.02852 =
0.02345 -0.00411 0.01274 -0.00333
C28 1 0.646261 -0.065865 0.511716 11.00000 0.03285 0.02842 =
0.02694 0.00039 0.01429 -0.00584
AFIX 43
H28 2 0.606588 -0.103354 0.518631 11.00000 -1.20000
AFIX 0
C29 1 0.723809 -0.092271 0.548202 11.00000 0.04008 0.02981 =
0.02403 0.00349 0.01120 -0.00131
AFIX 43
H29 2 0.737834 -0.147828 0.581073 11.00000 -1.20000
AFIX 0
C30 1 0.781971 -0.038821 0.537668 11.00000 0.03155 0.02914 =
0.02631 0.00107 0.00743 0.00289
AFIX 43
H30 2 0.835625 -0.058035 0.561705 11.00000 -1.20000
AFIX 0
C31 1 0.758694 0.043555 0.490765 11.00000 0.02529 0.02819 =
0.02351 0.00025 0.00827 -0.00091
C32 1 0.813172 0.110793 0.476827 11.00000 0.02507 0.03377 =
0.02413 0.00132 0.00926 0.00202
AFIX 43
H32 2 0.867789 0.096198 0.499127 11.00000 -1.20000
AFIX 0
C33 1 0.850383 0.258564 0.436457 11.00000 0.02852 0.02843 =
0.02869 0.00104 0.01126 -0.00288
C34 1 0.855786 0.279850 0.374832 11.00000 0.04018 0.03479 =
0.02886 0.00077 0.01360 -0.00407
C35 1 0.921157 0.337219 0.379644 11.00000 0.04221 0.03757 =
0.03276 -0.00128 0.02203 -0.00525
AFIX 43
H35 2 0.927575 0.351311 0.339227 11.00000 -1.20000
AFIX 0
C36 1 0.976868 0.374117 0.441715 11.00000 0.03054 0.03481 =
0.04794 -0.00453 0.01905 -0.00833
AFIX 43
H36 2 1.022206 0.409845 0.443895 11.00000 -1.20000
AFIX 0
C37 1 0.966639 0.359091 0.500278 11.00000 0.03234 0.03484 =
0.03191 -0.00225 0.00711 -0.00407
AFIX 43
H37 2 1.004262 0.387200 0.542342 11.00000 -1.20000
AFIX 0
C38 1 0.902137 0.303395 0.499318 11.00000 0.02807 0.03097 =
0.02805 -0.00176 0.00891 -0.00251
C39 1 0.890273 0.297316 0.564452 11.00000 0.03481 0.03844 =
0.02855 -0.00192 0.00930 -0.00361
AFIX 13
H39 2 0.839045 0.260913 0.552883 11.00000 -1.20000
AFIX 0
C40 1 0.885293 0.409023 0.591291 11.00000 0.04759 0.04275 =
0.03937 -0.00471 0.02410 -0.00177
AFIX 137
H40A 2 0.935884 0.445133 0.605645 11.00000 -1.50000
H40B 2 0.872367 0.402937 0.630419 11.00000 -1.50000
H40C 2 0.844454 0.450155 0.554904 11.00000 -1.50000
AFIX 0
C41 1 0.953860 0.233747 0.621432 11.00000 0.05396 0.04793 =
0.02912 0.00283 0.00980 0.00285
AFIX 137
H41A 2 0.954065 0.160558 0.605968 11.00000 -1.50000
H41B 2 0.943259 0.233361 0.661957 11.00000 -1.50000
H41C 2 1.005090 0.266499 0.632963 11.00000 -1.50000
AFIX 0
C42 1 0.794858 0.243081 0.305732 11.00000 0.04617 0.04415 =
0.02779 -0.00232 0.01638 -0.01651
AFIX 13
H42 2 0.751835 0.207837 0.313395 11.00000 -1.20000
AFIX 0
C43 1 0.825890 0.163458 0.272503 11.00000 0.09784 0.06440 =
0.05285 -0.02226 -0.01477 0.03708
AFIX 137
H43A 2 0.865760 0.196979 0.261303 11.00000 -1.50000
H43B 2 0.782910 0.137193 0.230482 11.00000 -1.50000
H43C 2 0.849385 0.103901 0.303899 11.00000 -1.50000
AFIX 0
C44 1 0.758981 0.335601 0.257916 11.00000 0.05366 0.05599 =
0.04246 -0.01308 -0.00036 0.01034
AFIX 137
H44A 2 0.741914 0.389760 0.281162 11.00000 -1.50000
H44B 2 0.713733 0.310774 0.217039 11.00000 -1.50000
H44C 2 0.798017 0.366302 0.244520 11.00000 -1.50000
AFIX 0
C45 1 0.912380 0.874883 0.714046 11.00000 0.05144 0.05179 =
0.03181 0.00292 0.00669 -0.00086
C46 1 0.928185 0.789242 0.682182 11.00000 0.04637 0.06307 =
0.03634 -0.00171 0.01756 0.00692
AFIX 43
H46 2 0.961898 0.798338 0.660285 11.00000 -1.20000
AFIX 0
C47 1 0.895618 0.689672 0.681525 11.00000 0.07389 0.05570 =
0.04593 -0.00455 0.01361 0.01090
AFIX 43
H47 2 0.906468 0.631436 0.658980 11.00000 -1.20000
AFIX 0
C48 1 0.848029 0.676902 0.713620 11.00000 0.06629 0.06731 =
0.04643 0.00686 0.01362 -0.01596
AFIX 43
H48 2 0.826084 0.609120 0.714130 11.00000 -1.20000
AFIX 0
C49 1 0.831679 0.761715 0.745241 11.00000 0.04278 0.08473 =
0.05485 0.00239 0.02343 -0.00072
AFIX 43
H49 2 0.798398 0.752320 0.767531 11.00000 -1.20000
AFIX 0
C50 1 0.862805 0.859192 0.744893 11.00000 0.05437 0.07337 =
0.04150 0.00069 0.02241 0.01075
AFIX 43
H50 2 0.850139 0.917397 0.766279 11.00000 -1.20000
AFIX 0
C51 1 0.948143 0.981279 0.715018 11.00000 0.10265 0.06521 =
0.05182 -0.00023 0.01881 -0.02113
AFIX 137
H51A 2 0.971920 0.981328 0.682715 11.00000 -1.50000
H51B 2 0.988531 0.996097 0.761211 11.00000 -1.50000
H51C 2 0.907421 1.036159 0.701765 11.00000 -1.50000
AFIX 6
PART -1
C52 1 1.096206 0.119212 0.561816 10.50000 0.13390
AFIX 137
H52A 2 1.113705 0.106689 0.610891 10.50000 -1.50000
H52B 2 1.076301 0.192027 0.550601 10.50000 -1.50000
H52C 2 1.140416 0.109308 0.550045 10.50000 -1.50000
AFIX 5
C53 1 1.031909 0.041708 0.521688 10.50000 0.06818
C58 1 1.014613 -0.044368 0.554049 10.50000 0.07873
AFIX 43
H58 2 1.043037 -0.052944 0.602132 10.50000 -1.20000
AFIX 5
C57 1 0.956315 -0.117689 0.516790 10.50000 0.06822
AFIX 43
H57 2 0.945432 -0.175559 0.539583 10.50000 -1.20000
AFIX 5
C56 1 0.913972 -0.106135 0.446090 10.50000 0.04928
AFIX 43
H56 2 0.874355 -0.156011 0.420622 10.50000 -1.20000
AFIX 5
C55 1 0.930358 -0.020638 0.413139 10.50000 0.06217
AFIX 43
H55 2 0.901739 -0.012166 0.365067 10.50000 -1.20000
AFIX 5
C54 1 0.988737 0.052433 0.450718 10.50000 0.04272
AFIX 43
H54 2 0.999368 0.110362 0.427811 10.50000 -1.20000
AFIX 0
HKLF 4
REM ila2_mg rigid group refinement
REM R1 = 0.0864 for 5486 Fo > 4sig(Fo) and 0.1845 for all 11395 data
REM 546 parameters refined using 0 restraints
END
WGHT 0.0658 0.0000
REM Highest difference peak 0.605, deepest hole -0.317, 1-sigma level 0.060
Q1 1 1.0117 0.0839 0.4600 11.00000 0.05 0.61
Q2 1 1.0379 -0.0132 0.5682 11.00000 0.05 0.49
Q3 1 0.9303 -0.1379 0.4958 11.00000 0.05 0.45
Q4 1 0.9095 -0.0585 0.4110 11.00000 0.05 0.39
Q5 1 1.1053 0.1879 0.5330 11.00000 0.05 0.32
Q6 1 1.0142 0.0128 0.5069 11.00000 0.05 0.31
Q7 1 0.6744 0.3174 0.3170 11.00000 0.05 0.25
Q8 1 0.6328 0.2453 0.3189 11.00000 0.05 0.23
Q9 1 0.8514 -0.1709 0.5970 11.00000 0.05 0.23
Q10 1 0.4597 0.5429 0.2266 11.00000 0.05 0.22
Q11 1 0.5758 0.1713 0.3538 11.00000 0.05 0.22
Q12 1 0.8015 0.1942 0.5415 11.00000 0.05 0.21
Q13 1 0.7884 -0.0735 0.3876 11.00000 0.05 0.20
Q14 1 0.7284 0.3085 0.4290 11.00000 0.05 0.20
Q15 1 1.0484 0.3608 0.4636 11.00000 0.05 0.20
Q16 1 0.4014 0.3218 0.1869 11.00000 0.05 0.20
Q17 1 0.5315 0.3085 0.1075 11.00000 0.05 0.20
Q18 1 0.7268 0.1640 0.3913 11.00000 0.05 0.19
Q19 1 0.6193 0.4131 0.1764 11.00000 0.05 0.19
Q20 1 0.8578 0.3278 0.2294 11.00000 0.05 0.19
Q21 1 0.9407 0.1543 0.3232 11.00000 0.05 0.19
Q22 1 0.4883 0.4735 0.5318 11.00000 0.05 0.19
Q23 1 0.5824 0.4377 0.1939 11.00000 0.05 0.19
Q24 1 0.8030 -0.2088 0.6484 11.00000 0.05 0.19
Q25 1 0.9054 0.3005 0.5293 11.00000 0.05 0.19
;
_shelx_res_checksum 89715
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
#######################################################################
#
# 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_zn11
_database_code_depnum_ccdc_archive 'CCDC 1554857'
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C95 H104 N12 Zn2'
_chemical_formula_weight 1544.64
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 2/c'
_space_group_name_Hall '-C 2yc'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 20.124(3)
_cell_length_b 19.606(3)
_cell_length_c 21.718(3)
_cell_angle_alpha 90
_cell_angle_beta 94.445(4)
_cell_angle_gamma 90
_cell_volume 8543(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 8974
_cell_measurement_theta_min 1.4521
_cell_measurement_theta_max 28.6902
_exptl_crystal_description prism
_exptl_crystal_colour orange
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.201
_exptl_crystal_F_000 3272
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.25
_exptl_absorpt_coefficient_mu 0.614
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.6135
_exptl_absorpt_process_details 'Blessing, 1995'
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source 'sealed tube'
_diffrn_measurement_device_type 'AFC7S Rigaku'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 33685
_diffrn_reflns_av_unetI/netI 0.1420
_diffrn_reflns_av_R_equivalents 0.1186
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 1.452
_diffrn_reflns_theta_max 28.691
_diffrn_reflns_theta_full 25.000
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total 9114
_reflns_number_gt 3939
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_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.
;
_computing_data_collection 'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution 'SIR2011 (Burla, 2012)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1559P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 9114
_refine_ls_number_parameters 482
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.2163
_refine_ls_R_factor_gt 0.0968
_refine_ls_wR_factor_ref 0.3286
_refine_ls_wR_factor_gt 0.2412
_refine_ls_goodness_of_fit_ref 0.999
_refine_ls_restrained_S_all 0.999
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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
Zn1 Zn 0.01747(3) 0.32987(4) 0.03094(4) 0.0612(3) Uani 1 1 d . . . . .
N1 N 0.1069(2) 0.3170(3) 0.0667(3) 0.0593(14) Uani 1 1 d . . . . .
N2 N 0.0622(2) 0.3327(2) -0.0525(3) 0.0560(13) Uani 1 1 d . . . . .
N3 N -0.0676(3) 0.3429(3) -0.1720(3) 0.0727(17) Uani 1 1 d . . . . .
N4 N -0.0540(3) 0.3921(3) 0.0457(3) 0.0673(15) Uani 1 1 d . . . . .
N5 N -0.0559(2) 0.2551(3) 0.0343(2) 0.0557(13) Uani 1 1 d . . . . .
N6 N 0.0225(2) 0.0950(3) 0.0135(3) 0.0668(15) Uani 1 1 d . . . . .
C1 C 0.1420(4) 0.3125(4) 0.1232(4) 0.076(2) Uani 1 1 d . . . . .
H1 H 0.1232 0.3103 0.1609 0.091 Uiso 1 1 calc R U . . .
C2 C 0.2092(4) 0.3119(4) 0.1155(4) 0.081(2) Uani 1 1 d . . . . .
H2 H 0.2434 0.3088 0.1467 0.097 Uiso 1 1 calc R U . . .
C3 C 0.2166(4) 0.3166(4) 0.0530(4) 0.076(2) Uani 1 1 d . . . . .
H3 H 0.2566 0.3172 0.0341 0.092 Uiso 1 1 calc R U . . .
C4 C 0.1534(3) 0.3203(3) 0.0240(3) 0.0603(17) Uani 1 1 d . . . . .
C5 C 0.1296(3) 0.3284(3) -0.0399(3) 0.0585(16) Uani 1 1 d . . . . .
C6 C 0.1714(3) 0.3305(4) -0.0894(4) 0.0674(18) Uani 1 1 d . . . . .
H6 H 0.2173 0.3266 -0.0815 0.081 Uiso 1 1 calc R U . . .
C7 C 0.1449(4) 0.3382(4) -0.1481(4) 0.078(2) Uani 1 1 d . . . . .
H7 H 0.1729 0.3411 -0.1801 0.093 Uiso 1 1 calc R U . . .
C8 C 0.0758(4) 0.3417(4) -0.1611(4) 0.072(2) Uani 1 1 d . . . . .
H8 H 0.0570 0.3455 -0.2014 0.087 Uiso 1 1 calc R U . . .
C9 C 0.0364(3) 0.3394(3) -0.1113(3) 0.0637(17) Uani 1 1 d . . . . .
C10 C -0.0378(3) 0.3425(3) -0.1201(4) 0.0629(17) Uani 1 1 d . . . . .
H10 H -0.0623 0.3442 -0.0855 0.076 Uiso 1 1 calc R U . . .
C11 C -0.1381(3) 0.3454(4) -0.1782(3) 0.0667(19) Uani 1 1 d . . . . .
C12 C -0.1742(4) 0.2837(5) -0.1829(4) 0.079(2) Uani 1 1 d . . . . .
C13 C -0.2431(4) 0.2876(6) -0.1919(4) 0.095(3) Uani 1 1 d . . . . .
H13 H -0.2680 0.2477 -0.1958 0.114 Uiso 1 1 calc R U . . .
C14 C -0.2749(4) 0.3488(6) -0.1950(4) 0.095(3) Uani 1 1 d . . . . .
H14 H -0.3212 0.3500 -0.1988 0.114 Uiso 1 1 calc R U . . .
C15 C -0.2401(4) 0.4080(5) -0.1926(4) 0.092(3) Uani 1 1 d . . . . .
H15 H -0.2631 0.4491 -0.1963 0.110 Uiso 1 1 calc R U . . .
C16 C -0.1707(4) 0.4091(4) -0.1849(4) 0.079(2) Uani 1 1 d . . . . .
C17 C -0.1329(4) 0.4743(5) -0.1817(5) 0.095(3) Uani 1 1 d . . . . .
H17 H -0.0876 0.4638 -0.1923 0.114 Uiso 1 1 calc R U . . .
C18 C -0.1609(6) 0.5268(7) -0.2284(6) 0.151(5) Uani 1 1 d . . . . .
H18A H -0.1604 0.5083 -0.2693 0.227 Uiso 1 1 calc R U . . .
H18B H -0.1340 0.5673 -0.2252 0.227 Uiso 1 1 calc R U . . .
H18C H -0.2058 0.5378 -0.2202 0.227 Uiso 1 1 calc R U . . .
C19 C -0.1268(5) 0.5040(6) -0.1173(5) 0.130(4) Uani 1 1 d . . . . .
H19A H -0.1696 0.5199 -0.1069 0.195 Uiso 1 1 calc R U . . .
H19B H -0.0960 0.5415 -0.1158 0.195 Uiso 1 1 calc R U . . .
H19C H -0.1109 0.4696 -0.0884 0.195 Uiso 1 1 calc R U . . .
C20 C -0.1383(5) 0.2149(5) -0.1808(5) 0.098(3) Uani 1 1 d . . . . .
H20 H -0.0922 0.2236 -0.1903 0.118 Uiso 1 1 calc R U . . .
C21 C -0.1355(7) 0.1847(6) -0.1197(5) 0.142(5) Uani 1 1 d . . . . .
H21A H -0.1234 0.2190 -0.0893 0.213 Uiso 1 1 calc R U . . .
H21B H -0.1028 0.1489 -0.1170 0.213 Uiso 1 1 calc R U . . .
H21C H -0.1783 0.1662 -0.1124 0.213 Uiso 1 1 calc R U . . .
C22 C -0.1668(10) 0.1626(8) -0.2272(6) 0.205(8) Uani 1 1 d . . . . .
H22A H -0.2074 0.1444 -0.2135 0.307 Uiso 1 1 calc R U . . .
H22B H -0.1353 0.1264 -0.2307 0.307 Uiso 1 1 calc R U . . .
H22C H -0.1759 0.1840 -0.2667 0.307 Uiso 1 1 calc R U . . .
C23 C -0.0648(4) 0.4582(4) 0.0587(4) 0.086(2) Uani 1 1 d . . . . .
H23 H -0.0326 0.4923 0.0595 0.103 Uiso 1 1 calc R U . . .
C24 C -0.1301(4) 0.4681(5) 0.0707(5) 0.095(3) Uani 1 1 d . . . . .
H24 H -0.1497 0.5095 0.0795 0.114 Uiso 1 1 calc R U . . .
C25 C -0.1608(4) 0.4067(5) 0.0674(4) 0.093(3) Uani 1 1 d . . . . .
H25 H -0.2050 0.3983 0.0746 0.111 Uiso 1 1 calc R U . . .
C26 C -0.1133(3) 0.3568(4) 0.0509(4) 0.072(2) Uani 1 1 d . . . . .
C27 C -0.1153(3) 0.2844(4) 0.0443(3) 0.0620(17) Uani 1 1 d . . . . .
C28 C -0.1716(3) 0.2442(4) 0.0497(3) 0.0673(18) Uani 1 1 d . . . . .
H28 H -0.2122 0.2647 0.0560 0.081 Uiso 1 1 calc R U . . .
C29 C -0.1676(3) 0.1771(4) 0.0459(4) 0.074(2) Uani 1 1 d . . . . .
H29 H -0.2055 0.1509 0.0499 0.089 Uiso 1 1 calc R U . . .
C30 C -0.1072(3) 0.1447(4) 0.0357(4) 0.0709(19) Uani 1 1 d . . . . .
H30 H -0.1039 0.0975 0.0326 0.085 Uiso 1 1 calc R U . . .
C31 C -0.0526(3) 0.1869(3) 0.0304(3) 0.0561(16) Uani 1 1 d . . . . .
C32 C 0.0141(3) 0.1582(3) 0.0197(3) 0.0562(16) Uani 1 1 d . . . . .
H32 H 0.0501 0.1875 0.0176 0.067 Uiso 1 1 calc R U . . .
C33 C 0.0875(3) 0.0700(3) 0.0038(3) 0.0620(17) Uani 1 1 d . . . . .
C34 C 0.1035(3) 0.0566(4) -0.0560(4) 0.0699(19) Uani 1 1 d . . . . .
C35 C 0.1675(4) 0.0300(4) -0.0625(4) 0.083(2) Uani 1 1 d . . . . .
H35 H 0.1805 0.0211 -0.1019 0.100 Uiso 1 1 calc R U . . .
C36 C 0.2115(4) 0.0167(4) -0.0124(5) 0.087(2) Uani 1 1 d . . . . .
H36 H 0.2536 -0.0005 -0.0182 0.104 Uiso 1 1 calc R U . . .
C37 C 0.1936(4) 0.0287(4) 0.0457(4) 0.087(2) Uani 1 1 d . . . . .
H37 H 0.2235 0.0187 0.0793 0.105 Uiso 1 1 calc R U . . .
C38 C 0.1313(3) 0.0557(3) 0.0558(4) 0.0672(18) Uani 1 1 d . . . . .
C39 C 0.1132(3) 0.0706(4) 0.1209(4) 0.077(2) Uani 1 1 d . . . . .
H39 H 0.0647 0.0761 0.1189 0.092 Uiso 1 1 calc R U . . .
C40 C 0.1309(5) 0.0126(6) 0.1667(5) 0.125(4) Uani 1 1 d . . . . .
H40A H 0.1075 -0.0280 0.1532 0.187 Uiso 1 1 calc R U . . .
H40B H 0.1182 0.0252 0.2069 0.187 Uiso 1 1 calc R U . . .
H40C H 0.1780 0.0044 0.1688 0.187 Uiso 1 1 calc R U . . .
C41 C 0.1432(5) 0.1375(6) 0.1438(5) 0.115(3) Uani 1 1 d . . . . .
H41A H 0.1908 0.1333 0.1491 0.173 Uiso 1 1 calc R U . . .
H41B H 0.1263 0.1490 0.1827 0.173 Uiso 1 1 calc R U . . .
H41C H 0.1314 0.1727 0.1143 0.173 Uiso 1 1 calc R U . . .
C42 C 0.0562(4) 0.0727(5) -0.1093(4) 0.091(2) Uani 1 1 d . . . . .
H42 H 0.0114 0.0684 -0.0950 0.109 Uiso 1 1 calc R U . . .
C43 C 0.0601(5) 0.0227(7) -0.1614(5) 0.131(4) Uani 1 1 d . . . . .
H43A H 0.1025 0.0269 -0.1784 0.196 Uiso 1 1 calc R U . . .
H43B H 0.0251 0.0321 -0.1929 0.196 Uiso 1 1 calc R U . . .
H43C H 0.0550 -0.0228 -0.1461 0.196 Uiso 1 1 calc R U . . .
C44 C 0.0620(6) 0.1445(6) -0.1323(5) 0.136(4) Uani 1 1 d . . . . .
H44A H 0.0662 0.1753 -0.0978 0.204 Uiso 1 1 calc R U . . .
H44B H 0.0229 0.1559 -0.1585 0.204 Uiso 1 1 calc R U . . .
H44C H 0.1007 0.1483 -0.1554 0.204 Uiso 1 1 calc R U . . .
C45 C 0.0000 0.2183(14) 0.2500 0.171(8) Uiso 1 2 d S . P . .
C46 C -0.0381(5) 0.2576(6) 0.2068(6) 0.125(3) Uiso 1 1 d . . . . .
H46 H -0.0651 0.2366 0.1757 0.151 Uiso 1 1 calc R U . . .
C47 C -0.0356(7) 0.3231(7) 0.2104(7) 0.149(5) Uiso 1 1 d . . . . .
H47 H -0.0633 0.3451 0.1804 0.178 Uiso 1 1 calc R U . . .
C48 C 0.0000 0.3672(14) 0.2500 0.176(8) Uiso 1 2 d S . P . .
H48 H 0.0000 0.4147 0.2500 0.211 Uiso 1 2 calc R U P . .
C49 C 0.0000 0.1527(16) 0.2500 0.228(12) Uiso 1 2 d S . P . .
H49A H -0.0296 0.1364 0.2164 0.342 Uiso 0.5 1 calc R U P . .
H49B H 0.0443 0.1364 0.2452 0.342 Uiso 0.5 1 calc R U P . .
H49C H -0.0147 0.1364 0.2884 0.342 Uiso 0.5 1 calc R U P . .
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
Zn1 0.0499(5) 0.0672(5) 0.0666(6) -0.0041(4) 0.0061(3) 0.0090(3)
N1 0.048(3) 0.062(3) 0.067(4) -0.002(3) 0.000(3) 0.004(2)
N2 0.044(3) 0.055(3) 0.069(4) -0.007(3) 0.006(2) 0.003(2)
N3 0.048(4) 0.105(5) 0.064(4) -0.001(3) -0.003(3) 0.005(3)
N4 0.057(3) 0.060(4) 0.085(4) -0.005(3) 0.007(3) 0.008(3)
N5 0.041(3) 0.071(4) 0.056(3) -0.003(3) 0.007(2) 0.007(2)
N6 0.056(3) 0.059(4) 0.086(4) 0.001(3) 0.009(3) 0.011(2)
C1 0.073(5) 0.085(5) 0.067(5) -0.007(4) -0.006(4) 0.008(4)
C2 0.070(5) 0.088(6) 0.080(6) -0.005(4) -0.020(4) 0.007(4)
C3 0.052(4) 0.076(5) 0.099(6) -0.008(4) -0.003(4) 0.011(3)
C4 0.046(4) 0.058(4) 0.077(5) -0.005(3) 0.002(3) 0.003(3)
C5 0.047(4) 0.062(4) 0.067(4) -0.003(3) 0.004(3) 0.006(3)
C6 0.049(4) 0.079(5) 0.075(5) -0.001(4) 0.010(3) 0.004(3)
C7 0.064(5) 0.090(6) 0.082(6) 0.006(4) 0.027(4) 0.002(3)
C8 0.067(5) 0.088(5) 0.062(4) 0.008(4) 0.009(3) 0.002(3)
C9 0.061(4) 0.060(4) 0.071(5) -0.004(3) 0.008(3) 0.007(3)
C10 0.047(4) 0.064(4) 0.077(5) -0.003(3) 0.005(3) 0.006(3)
C11 0.061(5) 0.090(6) 0.049(4) 0.002(3) 0.006(3) 0.002(4)
C12 0.073(5) 0.097(6) 0.066(5) 0.001(4) 0.005(4) -0.003(4)
C13 0.068(6) 0.142(9) 0.076(6) 0.001(5) 0.003(4) -0.020(5)
C14 0.062(5) 0.132(9) 0.089(6) 0.016(6) -0.006(4) 0.010(5)
C15 0.082(6) 0.109(7) 0.084(6) 0.007(5) 0.003(4) 0.027(5)
C16 0.068(5) 0.095(6) 0.072(5) 0.005(4) 0.000(4) 0.011(4)
C17 0.087(6) 0.075(6) 0.122(8) 0.000(5) 0.006(5) 0.010(4)
C18 0.186(11) 0.123(10) 0.141(11) 0.026(8) -0.003(9) -0.022(8)
C19 0.141(9) 0.106(8) 0.138(10) -0.015(7) -0.025(7) 0.004(6)
C20 0.104(6) 0.083(6) 0.108(8) 0.011(5) 0.014(5) -0.004(5)
C21 0.215(13) 0.128(10) 0.079(7) 0.003(7) -0.016(8) 0.054(9)
C22 0.38(3) 0.145(13) 0.081(8) -0.013(8) -0.040(12) 0.071(13)
C23 0.067(5) 0.072(5) 0.118(7) -0.021(5) 0.000(4) 0.015(4)
C24 0.074(5) 0.077(6) 0.134(8) -0.024(5) 0.013(5) 0.020(4)
C25 0.064(5) 0.082(6) 0.132(8) -0.015(5) 0.012(4) 0.024(4)
C26 0.050(4) 0.085(5) 0.081(5) -0.007(4) 0.009(3) 0.020(3)
C27 0.042(4) 0.081(5) 0.063(4) 0.002(3) 0.002(3) 0.014(3)
C28 0.045(4) 0.075(5) 0.082(5) -0.003(4) 0.006(3) 0.012(3)
C29 0.053(4) 0.081(6) 0.090(6) 0.006(4) 0.006(3) 0.001(3)
C30 0.056(4) 0.070(4) 0.088(5) 0.013(4) 0.011(3) 0.002(3)
C31 0.046(4) 0.068(4) 0.055(4) 0.000(3) 0.006(3) 0.008(3)
C32 0.047(4) 0.058(4) 0.063(4) 0.007(3) -0.001(3) 0.008(3)
C33 0.053(4) 0.051(4) 0.083(5) -0.004(3) 0.010(3) 0.007(3)
C34 0.061(4) 0.067(5) 0.083(5) 0.002(4) 0.013(4) 0.006(3)
C35 0.068(5) 0.081(5) 0.104(7) -0.012(4) 0.030(5) 0.002(4)
C36 0.048(4) 0.092(6) 0.121(8) -0.001(5) 0.008(5) 0.016(4)
C37 0.073(5) 0.082(6) 0.107(7) -0.005(5) 0.003(4) 0.020(4)
C38 0.062(4) 0.054(4) 0.086(5) 0.001(3) 0.004(4) 0.002(3)
C39 0.065(4) 0.085(5) 0.079(5) 0.004(4) 0.001(4) 0.002(4)
C40 0.141(8) 0.118(9) 0.116(8) 0.037(7) 0.014(7) 0.014(7)
C41 0.139(8) 0.120(8) 0.087(7) -0.021(6) 0.013(6) -0.009(7)
C42 0.091(6) 0.104(7) 0.078(6) -0.005(5) 0.007(4) 0.015(5)
C43 0.145(8) 0.170(12) 0.075(6) -0.032(7) 0.003(6) 0.004(8)
C44 0.179(11) 0.124(9) 0.108(9) 0.017(7) 0.030(8) 0.044(8)
_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
Zn1 N1 1.920(5) . ?
Zn1 N4 1.930(5) . ?
Zn1 N2 2.086(5) . ?
Zn1 N5 2.085(5) . ?
N1 C4 1.368(8) . ?
N1 C1 1.370(9) . ?
N2 C9 1.347(9) . ?
N2 C5 1.364(8) . ?
N3 C10 1.235(9) . ?
N3 C11 1.417(9) . ?
N4 C23 1.350(9) . ?
N4 C26 1.392(9) . ?
N5 C31 1.342(8) . ?
N5 C27 1.359(7) . ?
N6 C32 1.258(8) . ?
N6 C33 1.428(7) . ?
C1 C2 1.376(10) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.377(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.443(10) . ?
C5 C6 1.416(9) . ?
C6 C7 1.351(11) . ?
C6 H6 0.9300 . ?
C7 C8 1.399(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.391(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.491(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.411(11) . ?
C11 C16 1.412(11) . ?
C12 C13 1.387(11) . ?
C12 C20 1.529(12) . ?
C13 C14 1.358(14) . ?
C13 H13 0.9300 . ?
C14 C15 1.355(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.394(11) . ?
C15 H15 0.9300 . ?
C16 C17 1.488(12) . ?
C17 C19 1.510(14) . ?
C17 C18 1.522(15) . ?
C17 H17 0.9800 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.450(14) . ?
C20 C22 1.519(17) . ?
C20 H20 0.9800 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.373(10) . ?
C23 H23 0.9300 . ?
C24 C25 1.353(12) . ?
C24 H24 0.9300 . ?
C25 C26 1.432(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.426(11) . ?
C27 C28 1.393(9) . ?
C28 C29 1.322(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.404(9) . ?
C29 H29 0.9300 . ?
C30 C31 1.386(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.490(8) . ?
C32 H32 0.9300 . ?
C33 C34 1.386(10) . ?
C33 C38 1.407(10) . ?
C34 C35 1.407(9) . ?
C34 C42 1.478(11) . ?
C35 C36 1.372(11) . ?
C35 H35 0.9300 . ?
C36 C37 1.358(12) . ?
C36 H36 0.9300 . ?
C37 C38 1.394(9) . ?
C37 H37 0.9300 . ?
C38 C39 1.516(10) . ?
C39 C41 1.512(13) . ?
C39 C40 1.534(12) . ?
C39 H39 0.9800 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C44 1.501(14) . ?
C42 C43 1.504(13) . ?
C42 H42 0.9800 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C49 1.29(3) . ?
C45 C46 1.396(17) 2 ?
C45 C46 1.396(17) . ?
C46 C47 1.288(16) . ?
C46 H46 0.9300 . ?
C47 C48 1.381(19) . ?
C47 H47 0.9300 . ?
C48 C47 1.381(19) 2 ?
C48 H48 0.9300 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
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
N1 Zn1 N4 134.6(2) . . ?
N1 Zn1 N2 84.3(2) . . ?
N4 Zn1 N2 120.3(2) . . ?
N1 Zn1 N5 122.5(2) . . ?
N4 Zn1 N5 84.2(2) . . ?
N2 Zn1 N5 113.83(19) . . ?
C4 N1 C1 106.1(5) . . ?
C4 N1 Zn1 112.9(5) . . ?
C1 N1 Zn1 140.5(5) . . ?
C9 N2 C5 120.0(5) . . ?
C9 N2 Zn1 131.7(4) . . ?
C5 N2 Zn1 108.3(4) . . ?
C10 N3 C11 120.0(6) . . ?
C23 N4 C26 107.9(5) . . ?
C23 N4 Zn1 140.9(5) . . ?
C26 N4 Zn1 110.8(4) . . ?
C31 N5 C27 118.6(5) . . ?
C31 N5 Zn1 131.3(4) . . ?
C27 N5 Zn1 110.0(4) . . ?
C32 N6 C33 119.1(5) . . ?
N1 C1 C2 109.6(7) . . ?
N1 C1 H1 125.2 . . ?
C2 C1 H1 125.2 . . ?
C3 C2 C1 107.5(7) . . ?
C3 C2 H2 126.2 . . ?
C1 C2 H2 126.2 . . ?
C4 C3 C2 106.6(7) . . ?
C4 C3 H3 126.7 . . ?
C2 C3 H3 126.7 . . ?
N1 C4 C3 110.2(7) . . ?
N1 C4 C5 117.6(5) . . ?
C3 C4 C5 132.2(6) . . ?
N2 C5 C6 119.0(6) . . ?
N2 C5 C4 116.8(5) . . ?
C6 C5 C4 124.2(6) . . ?
C7 C6 C5 120.4(6) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C6 C7 C8 120.6(6) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C7 C8 C9 117.3(7) . . ?
C7 C8 H8 121.3 . . ?
C9 C8 H8 121.3 . . ?
N2 C9 C8 122.6(6) . . ?
N2 C9 C10 115.8(6) . . ?
C8 C9 C10 121.6(7) . . ?
N3 C10 C9 121.9(6) . . ?
N3 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C12 C11 C16 121.3(7) . . ?
C12 C11 N3 119.0(7) . . ?
C16 C11 N3 119.5(7) . . ?
C13 C12 C11 117.7(8) . . ?
C13 C12 C20 121.3(9) . . ?
C11 C12 C20 120.9(7) . . ?
C14 C13 C12 121.2(9) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 121.0(9) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C14 C15 C16 121.8(9) . . ?
C14 C15 H15 119.1 . . ?
C16 C15 H15 119.1 . . ?
C15 C16 C11 116.8(8) . . ?
C15 C16 C17 121.4(8) . . ?
C11 C16 C17 121.7(7) . . ?
C16 C17 C19 112.3(8) . . ?
C16 C17 C18 112.9(9) . . ?
C19 C17 C18 110.9(9) . . ?
C16 C17 H17 106.8 . . ?
C19 C17 H17 106.8 . . ?
C18 C17 H17 106.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C12 111.8(8) . . ?
C21 C20 C22 108.5(10) . . ?
C12 C20 C22 114.9(10) . . ?
C21 C20 H20 107.1 . . ?
C12 C20 H20 107.1 . . ?
C22 C20 H20 107.1 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 C24 110.3(7) . . ?
N4 C23 H23 124.8 . . ?
C24 C23 H23 124.8 . . ?
C25 C24 C23 107.8(7) . . ?
C25 C24 H24 126.1 . . ?
C23 C24 H24 126.1 . . ?
C24 C25 C26 108.1(7) . . ?
C24 C25 H25 126.0 . . ?
C26 C25 H25 126.0 . . ?
N4 C26 C25 106.0(7) . . ?
N4 C26 C27 120.1(5) . . ?
C25 C26 C27 133.7(7) . . ?
N5 C27 C28 120.4(6) . . ?
N5 C27 C26 114.8(6) . . ?
C28 C27 C26 124.8(5) . . ?
C29 C28 C27 120.3(6) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C28 C29 C30 121.2(7) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 H29 119.4 . . ?
C31 C30 C29 116.3(7) . . ?
C31 C30 H30 121.8 . . ?
C29 C30 H30 121.8 . . ?
N5 C31 C30 123.2(5) . . ?
N5 C31 C32 115.8(5) . . ?
C30 C31 C32 121.0(6) . . ?
N6 C32 C31 121.3(6) . . ?
N6 C32 H32 119.4 . . ?
C31 C32 H32 119.3 . . ?
C34 C33 C38 122.4(6) . . ?
C34 C33 N6 119.1(6) . . ?
C38 C33 N6 118.3(6) . . ?
C33 C34 C35 116.5(7) . . ?
C33 C34 C42 120.7(6) . . ?
C35 C34 C42 122.7(7) . . ?
C36 C35 C34 121.9(7) . . ?
C36 C35 H35 119.1 . . ?
C34 C35 H35 119.1 . . ?
C37 C36 C35 120.2(7) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C36 C37 C38 121.2(8) . . ?
C36 C37 H37 119.4 . . ?
C38 C37 H37 119.4 . . ?
C37 C38 C33 117.7(7) . . ?
C37 C38 C39 120.3(7) . . ?
C33 C38 C39 122.0(6) . . ?
C41 C39 C38 110.8(7) . . ?
C41 C39 C40 111.3(8) . . ?
C38 C39 C40 113.6(7) . . ?
C41 C39 H39 106.9 . . ?
C38 C39 H39 106.9 . . ?
C40 C39 H39 106.9 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C34 C42 C44 113.6(8) . . ?
C34 C42 C43 112.4(8) . . ?
C44 C42 C43 110.6(9) . . ?
C34 C42 H42 106.6 . . ?
C44 C42 H42 106.6 . . ?
C43 C42 H42 106.6 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C49 C45 C46 123.5(11) . 2 ?
C49 C45 C46 123.5(11) . . ?
C46 C45 C46 113(2) 2 . ?
C47 C46 C45 119.5(17) . . ?
C47 C46 H46 120.3 . . ?
C45 C46 H46 120.3 . . ?
C48 C47 C46 132.8(18) . . ?
C48 C47 H47 113.6 . . ?
C46 C47 H47 113.6 . . ?
C47 C48 C47 102(2) . 2 ?
C47 C48 H48 128.8 . . ?
C47 C48 H48 128.8 2 . ?
C45 C49 H49A 109.5 . . ?
C45 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C45 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 C1 C2 -1.0(8) . . . . ?
Zn1 N1 C1 C2 -171.8(6) . . . . ?
N1 C1 C2 C3 0.5(9) . . . . ?
C1 C2 C3 C4 0.2(9) . . . . ?
C1 N1 C4 C3 1.2(7) . . . . ?
Zn1 N1 C4 C3 174.8(5) . . . . ?
C1 N1 C4 C5 -177.4(6) . . . . ?
Zn1 N1 C4 C5 -3.7(7) . . . . ?
C2 C3 C4 N1 -0.9(8) . . . . ?
C2 C3 C4 C5 177.4(7) . . . . ?
C9 N2 C5 C6 -0.5(9) . . . . ?
Zn1 N2 C5 C6 -178.9(5) . . . . ?
C9 N2 C5 C4 -179.2(6) . . . . ?
Zn1 N2 C5 C4 2.4(6) . . . . ?
N1 C4 C5 N2 0.6(8) . . . . ?
C3 C4 C5 N2 -177.5(7) . . . . ?
N1 C4 C5 C6 -178.0(6) . . . . ?
C3 C4 C5 C6 3.9(12) . . . . ?
N2 C5 C6 C7 1.4(10) . . . . ?
C4 C5 C6 C7 180.0(7) . . . . ?
C5 C6 C7 C8 -2.2(11) . . . . ?
C6 C7 C8 C9 2.1(11) . . . . ?
C5 N2 C9 C8 0.5(10) . . . . ?
Zn1 N2 C9 C8 178.4(5) . . . . ?
C5 N2 C9 C10 179.0(5) . . . . ?
Zn1 N2 C9 C10 -3.1(9) . . . . ?
C7 C8 C9 N2 -1.2(10) . . . . ?
C7 C8 C9 C10 -179.7(6) . . . . ?
C11 N3 C10 C9 179.5(6) . . . . ?
N2 C9 C10 N3 -173.9(6) . . . . ?
C8 C9 C10 N3 4.6(10) . . . . ?
C10 N3 C11 C12 -92.2(9) . . . . ?
C10 N3 C11 C16 93.1(9) . . . . ?
C16 C11 C12 C13 -2.5(11) . . . . ?
N3 C11 C12 C13 -177.0(7) . . . . ?
C16 C11 C12 C20 175.1(7) . . . . ?
N3 C11 C12 C20 0.5(11) . . . . ?
C11 C12 C13 C14 -1.1(12) . . . . ?
C20 C12 C13 C14 -178.6(8) . . . . ?
C12 C13 C14 C15 3.5(14) . . . . ?
C13 C14 C15 C16 -2.2(14) . . . . ?
C14 C15 C16 C11 -1.4(12) . . . . ?
C14 C15 C16 C17 -179.4(9) . . . . ?
C12 C11 C16 C15 3.6(11) . . . . ?
N3 C11 C16 C15 178.2(7) . . . . ?
C12 C11 C16 C17 -178.4(8) . . . . ?
N3 C11 C16 C17 -3.8(11) . . . . ?
C15 C16 C17 C19 84.8(11) . . . . ?
C11 C16 C17 C19 -93.1(9) . . . . ?
C15 C16 C17 C18 -41.5(12) . . . . ?
C11 C16 C17 C18 140.6(9) . . . . ?
C13 C12 C20 C21 -84.7(12) . . . . ?
C11 C12 C20 C21 97.9(10) . . . . ?
C13 C12 C20 C22 39.6(13) . . . . ?
C11 C12 C20 C22 -137.8(10) . . . . ?
C26 N4 C23 C24 -1.8(10) . . . . ?
Zn1 N4 C23 C24 -172.9(7) . . . . ?
N4 C23 C24 C25 2.2(11) . . . . ?
C23 C24 C25 C26 -1.8(11) . . . . ?
C23 N4 C26 C25 0.6(9) . . . . ?
Zn1 N4 C26 C25 174.7(5) . . . . ?
C23 N4 C26 C27 -175.0(7) . . . . ?
Zn1 N4 C26 C27 -1.0(8) . . . . ?
C24 C25 C26 N4 0.7(10) . . . . ?
C24 C25 C26 C27 175.5(9) . . . . ?
C31 N5 C27 C28 -0.7(9) . . . . ?
Zn1 N5 C27 C28 -178.6(5) . . . . ?
C31 N5 C27 C26 177.0(6) . . . . ?
Zn1 N5 C27 C26 -0.9(7) . . . . ?
N4 C26 C27 N5 1.3(10) . . . . ?
C25 C26 C27 N5 -173.0(8) . . . . ?
N4 C26 C27 C28 178.9(7) . . . . ?
C25 C26 C27 C28 4.7(13) . . . . ?
N5 C27 C28 C29 0.8(11) . . . . ?
C26 C27 C28 C29 -176.7(8) . . . . ?
C27 C28 C29 C30 -0.7(12) . . . . ?
C28 C29 C30 C31 0.4(11) . . . . ?
C27 N5 C31 C30 0.5(9) . . . . ?
Zn1 N5 C31 C30 177.8(5) . . . . ?
C27 N5 C31 C32 -179.7(5) . . . . ?
Zn1 N5 C31 C32 -2.3(9) . . . . ?
C29 C30 C31 N5 -0.3(10) . . . . ?
C29 C30 C31 C32 179.8(6) . . . . ?
C33 N6 C32 C31 -179.6(6) . . . . ?
N5 C31 C32 N6 -178.0(6) . . . . ?
C30 C31 C32 N6 1.9(10) . . . . ?
C32 N6 C33 C34 -97.1(8) . . . . ?
C32 N6 C33 C38 87.2(8) . . . . ?
C38 C33 C34 C35 -2.5(10) . . . . ?
N6 C33 C34 C35 -178.0(6) . . . . ?
C38 C33 C34 C42 -179.7(7) . . . . ?
N6 C33 C34 C42 4.8(10) . . . . ?
C33 C34 C35 C36 1.3(11) . . . . ?
C42 C34 C35 C36 178.5(8) . . . . ?
C34 C35 C36 C37 0.5(13) . . . . ?
C35 C36 C37 C38 -1.2(13) . . . . ?
C36 C37 C38 C33 0.0(12) . . . . ?
C36 C37 C38 C39 -178.2(8) . . . . ?
C34 C33 C38 C37 1.9(10) . . . . ?
N6 C33 C38 C37 177.4(6) . . . . ?
C34 C33 C38 C39 -179.9(7) . . . . ?
N6 C33 C38 C39 -4.4(10) . . . . ?
C37 C38 C39 C41 80.1(9) . . . . ?
C33 C38 C39 C41 -98.1(9) . . . . ?
C37 C38 C39 C40 -46.2(10) . . . . ?
C33 C38 C39 C40 135.7(8) . . . . ?
C33 C34 C42 C44 87.0(10) . . . . ?
C35 C34 C42 C44 -90.1(9) . . . . ?
C33 C34 C42 C43 -146.5(8) . . . . ?
C35 C34 C42 C43 36.4(12) . . . . ?
C49 C45 C46 C47 179.4(9) . . . . ?
C46 C45 C46 C47 -0.6(9) 2 . . . ?
C45 C46 C47 C48 1(2) . . . . ?
C46 C47 C48 C47 -0.8(12) . . . 2 ?
_refine_diff_density_max 0.571
_refine_diff_density_min -0.999
_refine_diff_density_rms 0.122
_shelx_res_file
;
zn11.res created by SHELXL-2014/7
TITL zn_rt_10s
REM Shelx file produced by Sir2011 on Sat Apr 09 2016 at 09:02:52
REM Structure name: zn_rt_10s
CELL 0.71073 20.124 19.6057 21.7176 90 94.4446 90
ZERR 4 0.0029 0.0029 0.0031 0 0.004 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N Zn
UNIT 380 416 48 8
L.S. 15
PLAN 25
MPLA 14 N1 N2 N3 C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11
MPLA 14 N4 N5 N6 C23 C24 C25 C26 C27 C28 C29 C30 C31 C32 C33
MPLA 14 N1 N2 N3 C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 C11
MPLA 8 C11 C12 C13 C14 C15 C16 C17 C20
MPLA 14 N4 N5 N6 C23 C24 C25 C26 C27 C28 C29 C30 C31 C32 C33
MPLA 8 C33 C34 C35 C36 C37 C38 C39 C42
MORE -1
BOND $H
CONF
fmap 2
acta 50
REM
REM
REM
WGHT 0.155900
FVAR 0.55734
ZN1 4 0.017473 0.329870 0.030935 11.00000 0.04994 0.06716 =
0.06661 -0.00407 0.00612 0.00900
N1 3 0.106889 0.317000 0.066667 11.00000 0.04831 0.06170 =
0.06733 -0.00232 0.00021 0.00377
N2 3 0.062245 0.332728 -0.052488 11.00000 0.04435 0.05476 =
0.06925 -0.00687 0.00606 0.00299
N3 3 -0.067591 0.342913 -0.171984 11.00000 0.04764 0.10519 =
0.06411 -0.00064 -0.00285 0.00510
N4 3 -0.053965 0.392050 0.045654 11.00000 0.05724 0.05964 =
0.08539 -0.00482 0.00743 0.00806
N5 3 -0.055869 0.255128 0.034315 11.00000 0.04091 0.07057 =
0.05614 -0.00261 0.00661 0.00691
N6 3 0.022516 0.095016 0.013538 11.00000 0.05643 0.05875 =
0.08575 0.00079 0.00918 0.01129
C1 1 0.141956 0.312533 0.123190 11.00000 0.07252 0.08550 =
0.06694 -0.00662 -0.00595 0.00786
AFIX 43
H1 2 0.123191 0.310279 0.160946 11.00000 -1.20000
AFIX 0
C2 1 0.209169 0.311895 0.115511 11.00000 0.07020 0.08820 =
0.08043 -0.00545 -0.01999 0.00654
AFIX 43
H2 2 0.243359 0.308825 0.146749 11.00000 -1.20000
AFIX 0
C3 1 0.216637 0.316643 0.052981 11.00000 0.05212 0.07650 =
0.09923 -0.00805 -0.00252 0.01075
AFIX 43
H3 2 0.256569 0.317248 0.034111 11.00000 -1.20000
AFIX 0
C4 1 0.153412 0.320307 0.024043 11.00000 0.04553 0.05763 =
0.07738 -0.00542 0.00173 0.00303
C5 1 0.129576 0.328371 -0.039910 11.00000 0.04707 0.06187 =
0.06652 -0.00274 0.00443 0.00580
C6 1 0.171364 0.330486 -0.089393 11.00000 0.04919 0.07911 =
0.07484 -0.00066 0.01047 0.00372
AFIX 43
H6 2 0.217286 0.326578 -0.081460 11.00000 -1.20000
AFIX 0
C7 1 0.144905 0.338151 -0.148086 11.00000 0.06397 0.08983 =
0.08207 0.00617 0.02672 0.00224
AFIX 43
H7 2 0.172875 0.341061 -0.180124 11.00000 -1.20000
AFIX 0
C8 1 0.075792 0.341749 -0.161097 11.00000 0.06714 0.08843 =
0.06160 0.00786 0.00860 0.00153
AFIX 43
H8 2 0.056966 0.345531 -0.201431 11.00000 -1.20000
AFIX 0
C9 1 0.036397 0.339443 -0.111285 11.00000 0.06067 0.06018 =
0.07079 -0.00381 0.00765 0.00696
C10 1 -0.037775 0.342516 -0.120091 11.00000 0.04733 0.06418 =
0.07739 -0.00297 0.00541 0.00592
AFIX 43
H10 2 -0.062273 0.344181 -0.085528 11.00000 -1.20000
AFIX 0
C11 1 -0.138143 0.345366 -0.178222 11.00000 0.06056 0.09032 =
0.04941 0.00180 0.00641 0.00161
C12 1 -0.174232 0.283657 -0.182891 11.00000 0.07324 0.09727 =
0.06608 0.00132 0.00520 -0.00307
C13 1 -0.243108 0.287604 -0.191877 11.00000 0.06775 0.14190 =
0.07574 0.00092 0.00285 -0.01978
AFIX 43
H13 2 -0.267995 0.247659 -0.195844 11.00000 -1.20000
AFIX 0
C14 1 -0.274856 0.348788 -0.194985 11.00000 0.06202 0.13204 =
0.08860 0.01627 -0.00642 0.00952
AFIX 43
H14 2 -0.321190 0.350041 -0.198793 11.00000 -1.20000
AFIX 0
C15 1 -0.240075 0.408010 -0.192626 11.00000 0.08153 0.10883 =
0.08403 0.00662 0.00257 0.02652
AFIX 43
H15 2 -0.263136 0.449099 -0.196270 11.00000 -1.20000
AFIX 0
C16 1 -0.170655 0.409053 -0.184884 11.00000 0.06843 0.09494 =
0.07190 0.00513 -0.00049 0.01125
C17 1 -0.132899 0.474349 -0.181689 11.00000 0.08680 0.07540 =
0.12183 0.00039 0.00621 0.00974
AFIX 13
H17 2 -0.087576 0.463798 -0.192304 11.00000 -1.20000
AFIX 0
C18 1 -0.160884 0.526786 -0.228434 11.00000 0.18641 0.12334 =
0.14112 0.02554 -0.00314 -0.02154
AFIX 137
H18A 2 -0.160426 0.508341 -0.269347 11.00000 -1.50000
H18B 2 -0.134045 0.567298 -0.225217 11.00000 -1.50000
H18C 2 -0.205833 0.537797 -0.220226 11.00000 -1.50000
AFIX 0
C19 1 -0.126802 0.504033 -0.117327 11.00000 0.14133 0.10562 =
0.13765 -0.01457 -0.02487 0.00372
AFIX 137
H19A 2 -0.169642 0.519888 -0.106886 11.00000 -1.50000
H19B 2 -0.095993 0.541491 -0.115768 11.00000 -1.50000
H19C 2 -0.110894 0.469589 -0.088415 11.00000 -1.50000
AFIX 0
C20 1 -0.138286 0.214907 -0.180797 11.00000 0.10365 0.08269 =
0.10837 0.01095 0.01357 -0.00379
AFIX 13
H20 2 -0.092230 0.223609 -0.190300 11.00000 -1.20000
AFIX 0
C21 1 -0.135474 0.184711 -0.119727 11.00000 0.21485 0.12805 =
0.07884 0.00332 -0.01577 0.05369
AFIX 137
H21A 2 -0.123404 0.218982 -0.089323 11.00000 -1.50000
H21B 2 -0.102819 0.148924 -0.116981 11.00000 -1.50000
H21C 2 -0.178335 0.166228 -0.112430 11.00000 -1.50000
AFIX 0
C22 1 -0.166848 0.162600 -0.227184 11.00000 0.37946 0.14462 =
0.08121 -0.01298 -0.03987 0.07125
AFIX 137
H22A 2 -0.207447 0.144359 -0.213484 11.00000 -1.50000
H22B 2 -0.135273 0.126369 -0.230686 11.00000 -1.50000
H22C 2 -0.175876 0.184013 -0.266701 11.00000 -1.50000
AFIX 0
C23 1 -0.064767 0.458246 0.058742 11.00000 0.06708 0.07230 =
0.11768 -0.02120 0.00012 0.01489
AFIX 43
H23 2 -0.032568 0.492328 0.059540 11.00000 -1.20000
AFIX 0
C24 1 -0.130076 0.468079 0.070709 11.00000 0.07421 0.07658 =
0.13437 -0.02424 0.01290 0.01995
AFIX 43
H24 2 -0.149682 0.509544 0.079523 11.00000 -1.20000
AFIX 0
C25 1 -0.160804 0.406688 0.067389 11.00000 0.06440 0.08174 =
0.13239 -0.01515 0.01176 0.02446
AFIX 43
H25 2 -0.205036 0.398330 0.074562 11.00000 -1.20000
AFIX 0
C26 1 -0.113333 0.356820 0.050903 11.00000 0.04959 0.08515 =
0.08097 -0.00737 0.00877 0.02000
C27 1 -0.115258 0.284449 0.044345 11.00000 0.04181 0.08056 =
0.06324 0.00177 0.00182 0.01420
C28 1 -0.171593 0.244248 0.049714 11.00000 0.04512 0.07487 =
0.08223 -0.00271 0.00624 0.01192
AFIX 43
H28 2 -0.212186 0.264732 0.056043 11.00000 -1.20000
AFIX 0
C29 1 -0.167594 0.177125 0.045853 11.00000 0.05264 0.08080 =
0.09006 0.00579 0.00632 0.00141
AFIX 43
H29 2 -0.205484 0.150863 0.049946 11.00000 -1.20000
AFIX 0
C30 1 -0.107178 0.144725 0.035681 11.00000 0.05578 0.06952 =
0.08828 0.01331 0.01082 0.00167
AFIX 43
H30 2 -0.103939 0.097545 0.032647 11.00000 -1.20000
AFIX 0
C31 1 -0.052635 0.186912 0.030410 11.00000 0.04614 0.06763 =
0.05495 0.00036 0.00635 0.00796
C32 1 0.014064 0.158162 0.019725 11.00000 0.04738 0.05775 =
0.06251 0.00683 -0.00110 0.00808
AFIX 43
H32 2 0.050147 0.187474 0.017587 11.00000 -1.20000
AFIX 0
C33 1 0.087508 0.070045 0.003765 11.00000 0.05252 0.05085 =
0.08349 -0.00375 0.01042 0.00652
C34 1 0.103545 0.056553 -0.055950 11.00000 0.06138 0.06694 =
0.08260 0.00181 0.01302 0.00554
C35 1 0.167547 0.029972 -0.062505 11.00000 0.06804 0.08065 =
0.10447 -0.01179 0.03033 0.00213
AFIX 43
H35 2 0.180471 0.021114 -0.101916 11.00000 -1.20000
AFIX 0
C36 1 0.211453 0.016742 -0.012387 11.00000 0.04754 0.09169 =
0.12129 -0.00126 0.00776 0.01573
AFIX 43
H36 2 0.253568 -0.000475 -0.018216 11.00000 -1.20000
AFIX 0
C37 1 0.193625 0.028702 0.045700 11.00000 0.07283 0.08168 =
0.10692 -0.00503 0.00346 0.01985
AFIX 43
H37 2 0.223518 0.018724 0.079310 11.00000 -1.20000
AFIX 0
C38 1 0.131324 0.055664 0.055811 11.00000 0.06160 0.05404 =
0.08576 0.00089 0.00360 0.00240
C39 1 0.113194 0.070603 0.120935 11.00000 0.06499 0.08537 =
0.07939 0.00372 0.00113 0.00186
AFIX 13
H39 2 0.064668 0.076078 0.118915 11.00000 -1.20000
AFIX 0
C40 1 0.130863 0.012613 0.166716 11.00000 0.14064 0.11785 =
0.11606 0.03717 0.01439 0.01411
AFIX 137
H40A 2 0.107492 -0.028042 0.153171 11.00000 -1.50000
H40B 2 0.118150 0.025216 0.206871 11.00000 -1.50000
H40C 2 0.178006 0.004370 0.168758 11.00000 -1.50000
AFIX 0
C41 1 0.143156 0.137511 0.143822 11.00000 0.13927 0.11992 =
0.08669 -0.02119 0.01293 -0.00948
AFIX 137
H41A 2 0.190785 0.133287 0.149072 11.00000 -1.50000
H41B 2 0.126303 0.148992 0.182664 11.00000 -1.50000
H41C 2 0.131409 0.172746 0.114267 11.00000 -1.50000
AFIX 0
C42 1 0.056152 0.072743 -0.109338 11.00000 0.09073 0.10409 =
0.07760 -0.00519 0.00700 0.01493
AFIX 13
H42 2 0.011362 0.068396 -0.094985 11.00000 -1.20000
AFIX 0
C43 1 0.060055 0.022708 -0.161399 11.00000 0.14543 0.17021 =
0.07510 -0.03154 0.00277 0.00415
AFIX 137
H43A 2 0.102505 0.026887 -0.178395 11.00000 -1.50000
H43B 2 0.025141 0.032085 -0.192923 11.00000 -1.50000
H43C 2 0.055009 -0.022798 -0.146119 11.00000 -1.50000
AFIX 0
C44 1 0.062019 0.144534 -0.132340 11.00000 0.17902 0.12369 =
0.10809 0.01745 0.02969 0.04407
AFIX 137
H44A 2 0.066200 0.175273 -0.097849 11.00000 -1.50000
H44B 2 0.022940 0.155946 -0.158479 11.00000 -1.50000
H44C 2 0.100669 0.148291 -0.155401 11.00000 -1.50000
AFIX 0
C45 1 0.000000 0.218318 0.250000 10.50000 0.17056
C46 1 -0.038124 0.257587 0.206800 11.00000 0.12544
AFIX 43
H46 2 -0.065104 0.236589 0.175654 11.00000 -1.20000
AFIX 0
C47 1 -0.035626 0.323102 0.210435 11.00000 0.14871
AFIX 43
H47 2 -0.063345 0.345060 0.180425 11.00000 -1.20000
AFIX 0
C48 1 0.000000 0.367243 0.250000 10.50000 0.17573
AFIX 43
H48 2 0.000002 0.414679 0.249999 10.50000 -1.20000
AFIX 0
C49 1 0.000000 0.152681 0.250000 10.50000 0.22821
AFIX 33
H49A 2 -0.029617 0.136359 0.216437 10.50000 -1.50000
H49B 2 0.044278 0.136359 0.245202 10.50000 -1.50000
H49C 2 -0.014661 0.136359 0.288361 10.50000 -1.50000
AFIX 0
HKLF 4
REM zn_rt_10s
REM R1 = 0.0968 for 3939 Fo > 4sig(Fo) and 0.2163 for all 9114 data
REM 482 parameters refined using 0 restraints
END
WGHT 0.1454 0.0000
REM Highest difference peak 0.571, deepest hole -0.999, 1-sigma level 0.122
Q1 1 -0.0346 0.2021 0.2062 11.00000 0.05 0.57
Q2 1 -0.0958 0.1920 -0.2198 11.00000 0.05 0.46
Q3 1 -0.2793 0.2253 0.0429 11.00000 0.05 0.44
Q4 1 0.0198 0.0063 0.0284 11.00000 0.05 0.43
Q5 1 -0.0438 0.2939 0.2024 11.00000 0.05 0.41
Q6 1 -0.1662 0.0754 -0.2041 11.00000 0.05 0.39
Q7 1 0.1974 -0.0278 0.0514 11.00000 0.05 0.37
Q8 1 0.1597 0.0756 -0.1013 11.00000 0.05 0.36
Q9 1 0.0000 0.1108 -0.2500 10.50000 0.05 0.36
Q10 1 -0.1337 0.0996 -0.2269 11.00000 0.05 0.35
Q11 1 -0.0790 0.1172 -0.2352 11.00000 0.05 0.35
Q12 1 -0.1974 0.4235 0.0372 11.00000 0.05 0.35
Q13 1 0.0000 0.0648 -0.2500 10.50000 0.05 0.34
Q14 1 -0.0712 0.4554 0.1729 11.00000 0.05 0.34
Q15 1 0.1451 -0.0396 0.0617 11.00000 0.05 0.34
Q16 1 0.2991 -0.0781 -0.0435 11.00000 0.05 0.34
Q17 1 -0.0406 0.3654 0.2074 11.00000 0.05 0.33
Q18 1 0.2502 -0.0682 -0.0387 11.00000 0.05 0.33
Q19 1 -0.2224 0.4444 0.0426 11.00000 0.05 0.33
Q20 1 -0.2153 0.0816 -0.1905 11.00000 0.05 0.33
Q21 1 -0.1242 0.0646 -0.2209 11.00000 0.05 0.33
Q22 1 -0.0999 0.0833 -0.2478 11.00000 0.05 0.33
Q23 1 -0.2109 0.2490 0.0299 11.00000 0.05 0.32
Q24 1 -0.1076 0.0985 -0.0596 11.00000 0.05 0.32
Q25 1 -0.0562 0.0781 -0.0757 11.00000 0.05 0.32
;
_shelx_res_checksum 72166
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'