Deliberate boxes and accidental wheels.
Kaur, Gurpreet; Polson, Matthew I. J.; Hartshorn, Richard M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 4200–4206; doi:10.1039/c4dt03089c

data_7033681
_publ_section_title
;
 Deliberate boxes and accidental wheels.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4200
_journal_page_last               4206
_journal_paper_doi               10.1039/c4dt03089c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
'C280 H244.8 Cl2.6 N50 Ni10 O7.4, 17.4(Cl), 44(O)'
_chemical_formula_sum            'C280 H244.8 Cl20 N50 Ni10 O51.4'
_chemical_formula_weight         6428.54
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-03-28
_audit_creation_method
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Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4813)
;
_audit_update_record
;
2015-01-16 deposited with the CCDC.
2015-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                64.9465(18)
_cell_angle_beta                 85.1949(14)
_cell_angle_gamma                81.8728(13)
_cell_formula_units_Z            1
_cell_length_a                   16.7862(2)
_cell_length_b                   24.9108(4)
_cell_length_c                   26.1281(5)
_cell_measurement_reflns_used    48348
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      73.8530
_cell_measurement_theta_min      3.1880
_cell_volume                     9794.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.02(10)
_diffrn_detector_area_resol_mean 5.3250
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0297445000
_diffrn_orient_matrix_UB_12      0.0077432000
_diffrn_orient_matrix_UB_13      0.0504028000
_diffrn_orient_matrix_UB_21      0.0253366000
_diffrn_orient_matrix_UB_22      0.0613132000
_diffrn_orient_matrix_UB_23      -0.0405215000
_diffrn_orient_matrix_UB_31      -0.0841065000
_diffrn_orient_matrix_UB_32      0.0301003000
_diffrn_orient_matrix_UB_33      0.0075314000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            111735
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.866
_diffrn_reflns_theta_min         3.120
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.267
_exptl_absorpt_correction_T_max  1.264
_exptl_absorpt_correction_T_min  0.545
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'metallic pale green'
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_description       block
_exptl_crystal_F_000             3306
_exptl_crystal_size_max          0.3677
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.1418
_refine_diff_density_max         3.485
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1800
_refine_ls_number_reflns         38593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0801
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1585P)^2^+8.1798P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2399
_refine_ls_wR_factor_ref         0.2548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30559
_reflns_number_total             38593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03089c2.cif
_cod_data_source_block           gka57a
_cod_depositor_comments
'Adding full bibliography for 7033678--7033682.cif.'
_cod_original_formula_sum        'C280 H244.80 Cl20 N50 Ni10 O51.40'
_cod_database_code               7033681
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C280H460N50Ni10Cl20O120
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: Cl3(0.9) O11(0.7) H11A(0.7) H11B(0.7) Cl2(0.9) Cl5(0.7) Cl7(0.5)
 Cl8(0.5) Cl9(0.4) Cl10(0.4) Cl14(0.5) Cl13(0.6) Cl1C(0.3) Cl1D(0.5) Cl1E(0.5)
 Cl1G(0.3)
3.a Rotating group:
 O11(H11A,H11B), O20(H20A,H20B), O35(H35A,H35B), O56(H56A,H56B)
3.b Ternary CH refined with riding coordinates:
 N15(H15), N36(H36), N37(H37), N40(H40), N62(H62)
3.c Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C85(H85A,H85B), C93(H93A,H93B), C109(H10A,H10B), C113(H11C,
 H11D), C118(H11E,H11F), C123(H12A,H12B), C124(H12C,H12D), C150(H15A,H15B),
 C155(H15C,H15D)
3.d Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C51(H51), C57(H57), C59(H59), C70(H70), C74(H74),
 C75(H75), C76(H76), C77(H77), C78(H78), C84(H84), C86(H86), C87(H87), C89(H89),
  C92(H92), C94(H94), C95(H95), C98(H98), C100(H100), C102(H102), C107(H107),
 C108(H108), C111(H111), C112(H112), C115(H115), C116(H116), C119(H119),
 C120(H120), C121(H121), C122(H122), C125(H125), C126(H126), C127(H127),
 C128(H128), C131(H131), C132(H132), C134(H134), C135(H135), C136(H136),
 C137(H137), C139(H139), C140(H140), C141(H141), C142(H142), C143(H143),
 C144(H144), C145(H145), C146(H146), C148(H148), C149(H149), C152(H152),
 C153(H153), C157(H157), C158(H158), C159(H159), C161(H161), C162(H162),
 C163(H163), C164(H164), C165(H165), C166(H166), C168(H168), C170(H170),
 C171(H171), C172(H172), C175(H175), C176(H176), C177(H177), C178(H178),
 C179(H179), C181(H181), C182(H182), C183(H183), C186(H186), C188(H188),
 C190(H190), C191(H191), C193(H193), C194(H194), C197(H197), C199(H199),
 C202(H202), C205(H205), C210(H210), C218(H218), C219(H219), C226(H226),
 C227(H227), C6(H6)
;