# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_exp_1068
_database_code_depnum_ccdc_archive 'CCDC 1569895'
_audit_update_record             
;
2018-01-29 deposited with the CCDC.
2018-01-31 downloaded from the CCDC.
;
_audit_creation_date             2018-01-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H25 N7 Ni O5, H2 O'
_chemical_formula_sum            'C29 H24.50 N7 Ni O6'
_chemical_formula_weight         625.76
_chemical_absolute_configuration ?
_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'
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'
Ni Ni 0.3393 1.1124 '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           5
_space_group_name_H-M_alt        'I 1 2 1'
_space_group_name_Hall           'I 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   9.2283(9)
_cell_length_b                   15.0673(10)
_cell_length_c                   25.829(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.810(8)
_cell_angle_gamma                90
_cell_volume                     3549.0(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6840
_cell_measurement_temperature    287.4(4)
_cell_measurement_theta_max      23.3590
_cell_measurement_theta_min      3.8370
_shelx_estimated_absorpt_T_max   0.916
_shelx_estimated_absorpt_T_min   0.901
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1294
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23610
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.192
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      287.4(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00  11.00   1.00   35.00    --  -15.84 -77.00 120.00   94
  2  ω    -29.00  49.00   1.00   35.00    --  -15.84  57.00-180.00   78
  3  ω    -85.00  -4.00   1.00   35.00    --  -15.84 -38.00-150.00   81
  4  ω    -64.00 -28.00   1.00   35.00    --  -15.84 115.00 155.53   36
  5  ω    -70.00  -7.00   1.00   35.00    --  -15.84 -57.00   0.00   63
  6  ω    -35.00  52.00   1.00   35.00    --  -15.84  38.00  30.00   87
  7  ω    -60.00  -1.00   1.00   35.00    --  -15.84 -57.00 -90.00   59
  8  ω    -29.00  51.00   1.00   35.00    --  -15.84  57.00 -90.00   80
  9  ω    -15.00  56.00   1.00   35.00    --   16.78 -99.00 120.00   71
 10  ω     15.00  64.00   1.00   35.00    --   16.78-113.00   5.73   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0195847000
_diffrn_orient_matrix_UB_12      0.0387644000
_diffrn_orient_matrix_UB_13      0.0150377000
_diffrn_orient_matrix_UB_21      -0.0749999000
_diffrn_orient_matrix_UB_22      0.0079308000
_diffrn_orient_matrix_UB_23      0.0015190000
_diffrn_orient_matrix_UB_31      0.0064568000
_diffrn_orient_matrix_UB_32      -0.0255263000
_diffrn_orient_matrix_UB_33      0.0233154000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4785
_reflns_number_total             6231
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 
;
 Flack x determined using 1539 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6215
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0826
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1520P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2270
_refine_ls_wR_factor_ref         0.2468
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O2-C28
 1.24 with sigma of 0.01
 C28-O3
 1.24 with sigma of 0.01
 C29-O4
 1.24 with sigma of 0.01
 C29-O5
 1.24 with sigma of 0.01
 O4-O5 \\sim O2-O3
 with sigma of 0.02
3. Rigid bond restraints
 O2, O4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Free rotating group:
 O6(H6A,H6B)
5.b Rotating group:
 O1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
;
_atom_sites_solution_hydrogens   mixed
_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
Ni1 Ni 0.32179(9) 0.50885(6) 0.79025(3) 0.0553(2) Uani 1 1 d . . . . .
O1 O 0.3980(9) 0.4515(6) 0.8656(3) 0.137(3) Uani 1 1 d . . . . .
H1A H 0.4413 0.4918 0.8880 0.206 Uiso 1 1 d GR . . . .
H1B H 0.4695 0.4121 0.8645 0.206 Uiso 1 1 d GR . . . .
O2 O 0.2072(7) 0.6010(4) 0.8257(2) 0.0874(18) Uani 1 1 d D U . A 1
O3 O 0.0750(12) 0.6644(7) 0.8780(5) 0.243(6) Uani 1 1 d D . . . .
O4 O 0.4473(7) 0.4080(4) 0.7562(2) 0.0842(18) Uani 1 1 d D U . B 2
O5 O 0.565(2) 0.3481(15) 0.8302(4) 0.288(8) Uiso 1 1 d D . . . .
N1 N 0.2737(7) 0.5465(4) 0.4211(2) 0.0579(16) Uani 1 1 d . . . . .
N2 N 0.2088(6) 0.5896(4) 0.6334(2) 0.0523(15) Uani 1 1 d . . . . .
N3 N 0.2494(7) 0.5679(4) 0.7190(2) 0.0522(14) Uani 1 1 d . . . . .
N4 N 0.1366(6) 0.2076(4) 0.3354(2) 0.0526(15) Uani 1 1 d . . . . .
N5 N 0.0062(7) 0.0914(4) 0.3039(2) 0.0634(17) Uani 1 1 d . . . . .
N6 N 0.4921(7) 0.8223(4) 0.30736(19) 0.0550(15) Uani 1 1 d . . . . .
N7 N 0.6420(6) 0.9235(3) 0.2841(2) 0.0543(15) Uani 1 1 d . . . . .
C1 C 0.2557(8) 0.5580(5) 0.4748(3) 0.0559(18) Uani 1 1 d . . . . .
C2 C 0.2864(8) 0.4883(4) 0.5099(3) 0.0580(19) Uani 1 1 d . . . . .
H2 H 0.3230 0.4353 0.4987 0.070 Uiso 1 1 calc R . . . .
C3 C 0.2635(7) 0.4966(4) 0.5610(2) 0.0531(17) Uani 1 1 d . . . . .
H3 H 0.2762 0.4482 0.5837 0.064 Uiso 1 1 calc R . . . .
C4 C 0.2203(7) 0.5795(5) 0.5785(3) 0.0539(18) Uani 1 1 d . . . . .
C5 C 0.1888(8) 0.6488(5) 0.5453(3) 0.0560(18) Uani 1 1 d . . . . .
H5 H 0.1566 0.7026 0.5571 0.067 Uiso 1 1 calc R . . . .
C6 C 0.2062(8) 0.6370(5) 0.4922(3) 0.0604(19) Uani 1 1 d . . . . .
H6 H 0.1838 0.6836 0.4686 0.073 Uiso 1 1 calc R . . . .
C7 C 0.2818(8) 0.5431(5) 0.6738(3) 0.0559(19) Uani 1 1 d . . . . .
H7 H 0.3481 0.4980 0.6699 0.067 Uiso 1 1 calc R . . . .
C8 C 0.1219(10) 0.6485(5) 0.6551(3) 0.072(2) Uani 1 1 d . . . . .
H8 H 0.0574 0.6896 0.6373 0.087 Uiso 1 1 calc R . . . .
C9 C 0.1481(10) 0.6352(5) 0.7074(3) 0.072(2) Uani 1 1 d . . . . .
H9 H 0.1045 0.6666 0.7319 0.087 Uiso 1 1 calc R . . . .
C10 C 0.2380(7) 0.4627(4) 0.3972(2) 0.0468(16) Uani 1 1 d . . . . .
C11 C 0.3414(8) 0.4127(6) 0.3770(3) 0.070(2) Uani 1 1 d . . . . .
H11 H 0.4356 0.4351 0.3778 0.084 Uiso 1 1 calc R . . . .
C12 C 0.3071(8) 0.3298(5) 0.3556(3) 0.071(2) Uani 1 1 d . . . . .
H12 H 0.3771 0.2976 0.3412 0.085 Uiso 1 1 calc R . . . .
C13 C 0.1673(7) 0.2947(4) 0.3556(3) 0.0546(18) Uani 1 1 d . . . . .
C14 C 0.0656(7) 0.3432(5) 0.3757(3) 0.0557(18) Uani 1 1 d . . . . .
H14 H -0.0276 0.3199 0.3759 0.067 Uiso 1 1 calc R . . . .
C15 C 0.0989(8) 0.4275(5) 0.3959(3) 0.0582(19) Uani 1 1 d . . . . .
H15 H 0.0271 0.4606 0.4087 0.070 Uiso 1 1 calc R . . . .
C16 C 0.0013(8) 0.1771(4) 0.3170(3) 0.062(2) Uani 1 1 d . . . . .
H16 H -0.0839 0.2110 0.3139 0.075 Uiso 1 1 calc R . . . .
C17 C 0.2291(8) 0.1382(5) 0.3331(3) 0.068(2) Uani 1 1 d . . . . .
H17 H 0.3303 0.1389 0.3430 0.082 Uiso 1 1 calc R . . . .
C18 C 0.1482(9) 0.0687(5) 0.3141(4) 0.077(3) Uani 1 1 d . . . . .
H18 H 0.1850 0.0126 0.3088 0.093 Uiso 1 1 calc R . . . .
C19 C 0.3310(8) 0.6141(5) 0.3922(3) 0.0540(18) Uani 1 1 d . . . . .
C20 C 0.2934(9) 0.6210(5) 0.3390(3) 0.065(2) Uani 1 1 d . . . . .
H20 H 0.2302 0.5788 0.3216 0.077 Uiso 1 1 calc R . . . .
C21 C 0.3439(9) 0.6863(5) 0.3105(3) 0.065(2) Uani 1 1 d . . . . .
H21 H 0.3160 0.6888 0.2744 0.078 Uiso 1 1 calc R . . . .
C22 C 0.4390(8) 0.7499(4) 0.3364(3) 0.0521(17) Uani 1 1 d . . . . .
C23 C 0.4863(8) 0.7399(5) 0.3895(3) 0.067(2) Uani 1 1 d . . . . .
H23 H 0.5529 0.7802 0.4069 0.081 Uiso 1 1 calc R . . . .
C24 C 0.4363(8) 0.6713(5) 0.4168(3) 0.064(2) Uani 1 1 d . . . . .
H24 H 0.4735 0.6632 0.4520 0.077 Uiso 1 1 calc R . . . .
C25 C 0.6299(8) 0.8551(5) 0.3144(3) 0.065(2) Uani 1 1 d . . . . .
H25 H 0.7069 0.8318 0.3380 0.078 Uiso 1 1 calc R . . . .
C26 C 0.4095(10) 0.8730(6) 0.2709(3) 0.077(3) Uani 1 1 d . . . . .
H26 H 0.3103 0.8670 0.2579 0.093 Uiso 1 1 calc R . . . .
C27 C 0.5046(11) 0.9348(6) 0.2575(3) 0.083(3) Uani 1 1 d . . . . .
H27 H 0.4785 0.9795 0.2330 0.100 Uiso 1 1 calc R . . . .
C28 C 0.1381(11) 0.5995(7) 0.8605(4) 0.151(6) Uani 1 1 d D . . . .
H28 H 0.1296 0.5449 0.8767 0.181 Uiso 1 1 calc R . . A .
C29 C 0.516(2) 0.3491(10) 0.7822(4) 0.320(16) Uiso 1 1 d D . . . .
H29 H 0.5327 0.2982 0.7638 0.384 Uiso 1 1 calc R . . B .
O6 O 0.1761(4) 0.8014(3) 0.8386(2) 0.0621(13) Uani 1 1 d . . . . .
H6A H 0.2197 0.8410 0.8587 0.093 Uiso 1 1 d G . . . .
H6B H 0.2281 0.7879 0.8153 0.093 Uiso 1 1 d G . . . .


_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
Ni1 O1 2.148(8) . ?
Ni1 O2 2.044(6) . ?
Ni1 O4 2.176(6) . ?
Ni1 N3 2.061(5) . ?
Ni1 N5 2.094(6) 3 ?
Ni1 N7 2.085(6) 3_445 ?
O1 H1A 0.8898 . ?
O1 H1B 0.8916 . ?
O2 C28 1.181(10) . ?
O3 C28 1.257(10) . ?
O4 C29 1.227(11) . ?
O5 C29 1.255(11) . ?
N1 C1 1.432(9) . ?
N1 C10 1.422(8) . ?
N1 C19 1.413(9) . ?
N2 C4 1.446(9) . ?
N2 C7 1.349(8) . ?
N2 C8 1.373(10) . ?
N3 C7 1.303(9) . ?
N3 C9 1.380(10) . ?
N4 C13 1.424(9) . ?
N4 C16 1.347(9) . ?
N4 C17 1.357(10) . ?
N5 Ni1 2.094(6) 3_444 ?
N5 C16 1.338(9) . ?
N5 C18 1.340(10) . ?
N6 C22 1.451(8) . ?
N6 C25 1.350(9) . ?
N6 C26 1.354(10) . ?
N7 Ni1 2.085(6) 3_554 ?
N7 C25 1.311(9) . ?
N7 C27 1.357(11) . ?
C1 C2 1.388(10) . ?
C1 C6 1.374(11) . ?
C2 H2 0.9300 . ?
C2 C3 1.375(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.406(10) . ?
C4 C5 1.354(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.418(10) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C8 C9 1.350(11) . ?
C9 H9 0.9300 . ?
C10 C11 1.380(10) . ?
C10 C15 1.385(9) . ?
C11 H11 0.9300 . ?
C11 C12 1.382(11) . ?
C12 H12 0.9300 . ?
C12 C13 1.395(10) . ?
C13 C14 1.354(10) . ?
C14 H14 0.9300 . ?
C14 C15 1.390(10) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C17 C18 1.335(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.369(9) . ?
C19 C24 1.379(10) . ?
C20 H20 0.9300 . ?
C20 C21 1.353(11) . ?
C21 H21 0.9300 . ?
C21 C22 1.398(10) . ?
C22 C23 1.382(10) . ?
C23 H23 0.9300 . ?
C23 C24 1.371(11) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C26 C27 1.359(12) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
O6 H6A 0.8503 . ?
O6 H6B 0.8498 . ?

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
O1 Ni1 O4 88.0(3) . . ?
O2 Ni1 O1 89.3(3) . . ?
O2 Ni1 N3 89.3(2) . . ?
O2 Ni1 N5 89.1(3) . 3 ?
O2 Ni1 N7 89.6(2) . 3_445 ?
N3 Ni1 O1 178.1(3) . . ?
N3 Ni1 O4 93.5(2) . . ?
N3 Ni1 N5 92.2(2) . 3 ?
N3 Ni1 N7 93.0(2) . 3_445 ?
N5 Ni1 O1 86.7(3) 3 . ?
N5 Ni1 O4 90.8(2) 3 . ?
N7 Ni1 O1 88.1(3) 3_445 . ?
N7 Ni1 O4 90.3(2) 3_445 . ?
N7 Ni1 N5 174.6(2) 3_445 3 ?
Ni1 O1 H1A 111.5 . . ?
Ni1 O1 H1B 112.3 . . ?
H1A O1 H1B 102.4 . . ?
C28 O2 Ni1 134.8(7) . . ?
C29 O4 Ni1 122.9(8) . . ?
C10 N1 C1 118.4(5) . . ?
C19 N1 C1 122.2(5) . . ?
C19 N1 C10 119.3(5) . . ?
C7 N2 C4 127.0(6) . . ?
C7 N2 C8 105.9(6) . . ?
C8 N2 C4 127.2(6) . . ?
C7 N3 Ni1 126.0(5) . . ?
C7 N3 C9 104.9(6) . . ?
C9 N3 Ni1 128.8(5) . . ?
C16 N4 C13 124.5(6) . . ?
C16 N4 C17 106.1(6) . . ?
C17 N4 C13 129.4(6) . . ?
C16 N5 Ni1 123.9(5) . 3_444 ?
C16 N5 C18 105.5(6) . . ?
C18 N5 Ni1 128.8(5) . 3_444 ?
C25 N6 C22 126.2(6) . . ?
C25 N6 C26 107.8(6) . . ?
C26 N6 C22 125.8(6) . . ?
C25 N7 Ni1 125.4(5) . 3_554 ?
C25 N7 C27 104.0(6) . . ?
C27 N7 Ni1 129.2(5) . 3_554 ?
C2 C1 N1 119.8(6) . . ?
C6 C1 N1 120.9(6) . . ?
C6 C1 C2 119.2(6) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 C1 120.8(6) . . ?
C3 C2 H2 119.6 . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 118.8(6) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 N2 118.4(6) . . ?
C5 C4 N2 119.9(6) . . ?
C5 C4 C3 121.8(6) . . ?
C4 C5 H5 121.0 . . ?
C4 C5 C6 118.1(7) . . ?
C6 C5 H5 121.0 . . ?
C1 C6 C5 121.1(7) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
N2 C7 H7 123.6 . . ?
N3 C7 N2 112.8(6) . . ?
N3 C7 H7 123.6 . . ?
N2 C8 H8 126.7 . . ?
C9 C8 N2 106.7(7) . . ?
C9 C8 H8 126.7 . . ?
N3 C9 H9 125.1 . . ?
C8 C9 N3 109.7(7) . . ?
C8 C9 H9 125.1 . . ?
C11 C10 N1 121.5(6) . . ?
C11 C10 C15 118.3(6) . . ?
C15 C10 N1 120.2(6) . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 121.0(7) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.9(7) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 N4 118.9(6) . . ?
C14 C13 N4 121.8(6) . . ?
C14 C13 C12 119.4(7) . . ?
C13 C14 H14 119.6 . . ?
C13 C14 C15 120.7(6) . . ?
C15 C14 H14 119.6 . . ?
C10 C15 C14 120.7(7) . . ?
C10 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
N4 C16 H16 124.7 . . ?
N5 C16 N4 110.7(7) . . ?
N5 C16 H16 124.7 . . ?
N4 C17 H17 126.3 . . ?
C18 C17 N4 107.5(7) . . ?
C18 C17 H17 126.3 . . ?
N5 C18 H18 124.8 . . ?
C17 C18 N5 110.3(7) . . ?
C17 C18 H18 124.8 . . ?
C20 C19 N1 121.9(6) . . ?
C20 C19 C24 117.9(7) . . ?
C24 C19 N1 120.0(6) . . ?
C19 C20 H20 118.5 . . ?
C21 C20 C19 123.0(7) . . ?
C21 C20 H20 118.5 . . ?
C20 C21 H21 120.6 . . ?
C20 C21 C22 118.9(7) . . ?
C22 C21 H21 120.6 . . ?
C21 C22 N6 120.4(6) . . ?
C23 C22 N6 121.0(6) . . ?
C23 C22 C21 118.6(6) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.9(7) . . ?
C24 C23 H23 119.6 . . ?
C19 C24 H24 119.9 . . ?
C23 C24 C19 120.2(6) . . ?
C23 C24 H24 119.9 . . ?
N6 C25 H25 124.1 . . ?
N7 C25 N6 111.8(6) . . ?
N7 C25 H25 124.1 . . ?
N6 C26 H26 127.8 . . ?
N6 C26 C27 104.3(7) . . ?
C27 C26 H26 127.8 . . ?
N7 C27 C26 112.0(7) . . ?
N7 C27 H27 124.0 . . ?
C26 C27 H27 124.0 . . ?
O2 C28 O3 126.3(12) . . ?
O2 C28 H28 116.9 . . ?
O3 C28 H28 116.9 . . ?
O4 C29 O5 129.1(16) . . ?
O4 C29 H29 115.5 . . ?
O5 C29 H29 115.5 . . ?
H6A O6 H6B 109.5 . . ?

_olex2_date_sample_data_collection 2018-01-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.911
_oxdiff_exptl_absorpt_empirical_full_min 0.451
####################################################################### 
# 
# 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_k-2811-jh_sqd
_database_code_depnum_ccdc_archive 'CCDC 1571392'
_audit_update_record             
;
2018-01-29 deposited with the CCDC.
2018-01-31 downloaded from the CCDC.
;
_audit_creation_date             2018-01-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H42 Cd1 N14'
_chemical_formula_sum            'C54 H42 Cd N14'
_chemical_formula_weight         999.41
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   16.5393(6)
_cell_length_b                   16.5393(6)
_cell_length_c                   21.597(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5116.3(6)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    3674
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.0860
_cell_measurement_theta_min      3.7420
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.945
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.973
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.413
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.0584
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1600
_reflns_number_total             2016
_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 > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2010
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0941
_refine_ls_restrained_S_all      1.124
_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/[σ²(Fo²)+(0.0942P)²+30.4672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2104
_refine_ls_wR_factor_ref         0.2252
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C8(H8), C2(H2), C9(H9), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Cd1 Cd 1.0000 1.0000 0.5000 0.0704(6) Uani 1 6 d S T P . .
N3 N 0.3333 0.6667 0.4216(6) 0.088(3) Uani 1 3 d S T P . .
N2 N 0.7199(3) 0.9120(3) 0.4186(3) 0.0732(16) Uani 1 1 d . . . . .
N1 N 0.8689(3) 0.9710(3) 0.4412(3) 0.0797(17) Uani 1 1 d . . . . .
C4 C 0.6224(4) 0.8481(4) 0.4176(3) 0.0716(19) Uani 1 1 d . . . . .
C7 C 0.4313(4) 0.7279(4) 0.4204(4) 0.080(2) Uani 1 1 d . . . . .
C1 C 0.7866(4) 0.8982(4) 0.4433(4) 0.078(2) Uani 1 1 d . . . . .
H1 H 0.7746 0.8415 0.4602 0.093 Uiso 1 1 calc R . . . .
C3 C 0.7641(6) 1.0017(5) 0.3971(5) 0.120(4) Uani 1 1 d . . . . .
H3 H 0.7376 1.0330 0.3775 0.144 Uiso 1 1 calc R . . . .
C8 C 0.4701(5) 0.8020(7) 0.3846(6) 0.146(5) Uani 1 1 d . . . . .
H8 H 0.4325 0.8141 0.3587 0.176 Uiso 1 1 calc R . . . .
C2 C 0.8546(6) 1.0345(5) 0.4107(5) 0.119(3) Uani 1 1 d . . . . .
H2 H 0.9022 1.0941 0.4004 0.143 Uiso 1 1 calc R . . . .
C9 C 0.5653(5) 0.8622(7) 0.3843(5) 0.140(5) Uani 1 1 d . . . . .
H9 H 0.5895 0.9151 0.3593 0.168 Uiso 1 1 calc R . . . .
C5 C 0.5835(6) 0.7743(6) 0.4564(8) 0.189(7) Uani 1 1 d . . . . .
H5 H 0.6207 0.7653 0.4847 0.226 Uiso 1 1 calc R . . . .
C6 C 0.4884(6) 0.7118(6) 0.4544(7) 0.171(6) Uani 1 1 d . . . . .
H6 H 0.4639 0.6572 0.4775 0.205 Uiso 1 1 calc R . . . .


_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
Cd1 N1 2.346(5) . ?
Cd1 N1 2.346(5) 2_765 ?
Cd1 N1 2.346(5) 11_566 ?
Cd1 N1 2.346(5) 3_675 ?
Cd1 N1 2.346(5) 12_656 ?
Cd1 N1 2.346(5) 10_776 ?
N3 C7 1.418(6) . ?
N3 C7 1.418(6) 2_665 ?
N3 C7 1.418(6) 3_565 ?
N2 C4 1.420(7) . ?
N2 C1 1.344(8) . ?
N2 C3 1.366(8) . ?
N1 C1 1.291(7) . ?
N1 C2 1.356(10) . ?
C4 C9 1.298(10) . ?
C4 C5 1.350(12) . ?
C7 C8 1.313(11) . ?
C7 C6 1.323(11) . ?
C1 H1 0.9300 . ?
C3 H3 0.9300 . ?
C3 C2 1.346(11) . ?
C8 H8 0.9300 . ?
C8 C9 1.379(11) . ?
C2 H2 0.9300 . ?
C9 H9 0.9300 . ?
C5 H5 0.9300 . ?
C5 C6 1.385(11) . ?
C6 H6 0.9300 . ?

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 Cd1 N1 180.0(3) . 10_776 ?
N1 Cd1 N1 86.5(2) 2_765 12_656 ?
N1 Cd1 N1 86.5(2) . 12_656 ?
N1 Cd1 N1 93.5(2) 11_566 12_656 ?
N1 Cd1 N1 86.5(2) 11_566 3_675 ?
N1 Cd1 N1 93.5(2) 2_765 3_675 ?
N1 Cd1 N1 93.5(2) . 2_765 ?
N1 Cd1 N1 86.5(2) . 11_566 ?
N1 Cd1 N1 86.5(2) 10_776 2_765 ?
N1 Cd1 N1 93.5(2) . 3_675 ?
N1 Cd1 N1 180.0(3) 11_566 2_765 ?
N1 Cd1 N1 93.5(2) 10_776 11_566 ?
N1 Cd1 N1 86.5(2) 10_776 3_675 ?
N1 Cd1 N1 93.5(2) 10_776 12_656 ?
N1 Cd1 N1 180.0 12_656 3_675 ?
C7 N3 C7 119.96(5) 2_665 3_565 ?
C7 N3 C7 119.96(5) 2_665 . ?
C7 N3 C7 119.97(4) 3_565 . ?
C1 N2 C4 127.1(5) . . ?
C1 N2 C3 106.3(5) . . ?
C3 N2 C4 126.5(5) . . ?
C1 N1 Cd1 127.4(5) . . ?
C1 N1 C2 103.2(6) . . ?
C2 N1 Cd1 127.2(4) . . ?
C9 C4 N2 122.1(6) . . ?
C9 C4 C5 116.6(7) . . ?
C5 C4 N2 121.0(6) . . ?
C8 C7 N3 121.9(7) . . ?
C8 C7 C6 116.7(7) . . ?
C6 C7 N3 121.4(7) . . ?
N2 C1 H1 123.2 . . ?
N1 C1 N2 113.5(6) . . ?
N1 C1 H1 123.2 . . ?
N2 C3 H3 127.9 . . ?
C2 C3 N2 104.3(6) . . ?
C2 C3 H3 127.9 . . ?
C7 C8 H8 119.1 . . ?
C7 C8 C9 121.8(8) . . ?
C9 C8 H8 119.1 . . ?
N1 C2 H2 123.7 . . ?
C3 C2 N1 112.6(6) . . ?
C3 C2 H2 123.7 . . ?
C4 C9 C8 122.5(8) . . ?
C4 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.3(9) . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 121.8(8) . . ?
C7 C6 H6 119.1 . . ?
C5 C6 H6 119.1 . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.017 -0.011 -0.001 2372 638 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
