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_7033680
_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 H245.8 Br2.1 N50 Ni10 O7.9, 17.9(Br), 46(O)'
_chemical_formula_sum            'C280 H245.8 Br20 N50 Ni10 O53.9'
_chemical_formula_weight         7358.75
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-28
_audit_creation_method
;
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                65.062(3)
_cell_angle_beta                 85.547(2)
_cell_angle_gamma                82.033(2)
_cell_formula_units_Z            1
_cell_length_a                   16.9013(4)
_cell_length_b                   25.0753(7)
_cell_length_c                   26.0861(7)
_cell_measurement_reflns_used    31661
_cell_measurement_temperature    286.13(10)
_cell_measurement_theta_max      73.8040
_cell_measurement_theta_min      3.0770
_cell_volume                     9925.6(5)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
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      286.13(10)
_diffrn_detector_area_resol_mean 21.3001
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
  1 omega -114.00  -10.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313  -57.0000  -30.0000 104

  2 omega  -11.00   15.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313   38.0000 -150.0000 26

  3 omega -116.00  -16.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313  -38.0000 -150.0000 100

  4 omega  -92.00   -4.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313  125.0000  120.0000 88

  5 omega  -47.00   35.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313   38.0000  120.0000 82

  6 omega   48.00   86.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0313 -125.0000   30.0000 38

  7 omega   28.00  104.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000   30.0000 76

  8 omega   43.00   91.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000 -150.0000 48

  9 omega   30.00   91.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000    0.0000 61

 10 omega   79.00  117.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -125.0000  -30.0000 38

 11 omega   47.00  141.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -77.0000   60.0000 94

 12 omega   30.00   85.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  -90.0000 55

 13 omega   90.00  177.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000  -90.0000 87

 14 omega   61.00   89.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000   30.0000 28

 15 omega   96.00  111.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -125.0000 -150.0000 15

 16 omega   30.00   73.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  150.0000 43

 17 omega   77.00  178.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000 -180.0000 101

 18 omega   36.00  108.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -77.0000  -90.0000 72

 19 omega   81.00  141.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -77.0000  120.0000 60

 20 omega -114.00  -10.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313  -57.0000   90.0000 104

 21 omega -119.00   -6.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313  -77.0000 -150.0000 113

 22 omega  -50.00   36.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.0313   38.0000 -120.0000 86

 23 omega    1.00   82.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0313  -99.0000   90.0000 81

 24 omega    1.00   82.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0313  -99.0000  -30.0000 81
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0164326000
_diffrn_orient_matrix_UB_12      -0.0403065000
_diffrn_orient_matrix_UB_13      -0.0316934000
_diffrn_orient_matrix_UB_21      -0.0365219000
_diffrn_orient_matrix_UB_22      0.0506928000
_diffrn_orient_matrix_UB_23      -0.0536798000
_diffrn_orient_matrix_UB_31      0.0828927000
_diffrn_orient_matrix_UB_32      0.0214516000
_diffrn_orient_matrix_UB_33      -0.0189148000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            89188
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        73.500
_diffrn_reflns_theta_max         73.500
_diffrn_reflns_theta_min         2.640
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.365
_exptl_absorpt_correction_T_max  1.468
_exptl_absorpt_correction_T_min  0.637
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3687
_exptl_crystal_size_max          0.3128
_exptl_crystal_size_mid          0.1667
_exptl_crystal_size_min          0.0883
_refine_diff_density_max         5.591
_refine_diff_density_min         -2.162
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.366
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1828
_refine_ls_number_reflns         38714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.366
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.1000
_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^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3087
_refine_ls_wR_factor_ref         0.3323
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29908
_reflns_number_total             38714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03089c2.cif
_cod_data_source_block           gka39a
_cod_depositor_comments
'Adding full bibliography for 7033678--7033682.cif.'
_cod_original_formula_sum        'C280 H245.80 Br20 N50 Ni10 O53.90'
_cod_database_code               7033680
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C140H245N25NI5BR5O60
_reflns_odcompleteness_completeness 99.68
_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: Br3(0.9) Br17(0.5) Br4(0.4) O72(0.95) H72A(0.95) H72B(0.95)
 Br19(0.9) Br6(0.8) Br7(0.4) Br8(0.3) Br9(0.3) Br39(0.3) Br10(0.25) Br14(0.3)
 Br12(0.3) Br73(0.05) Br13(0.3)
3.a Rotating group:
 O72(H72A,H72B), O109(H10A,H10B), O144(H14A,H14B), O38(H38A,H38B)
3.b Ternary CH refined with riding coordinates:
 N100(H100), N63(H63), N135(H135), N29(H29), N171(H171)
3.c Secondary CH2 refined with riding coordinates:
 C134(H13A,H13B), C99(H99A,H99B), C62(H62A,H62B), C170(H17A,H17B), C172(H17C,
 H17D), C28(H28A,H28B), C101(H10C,H10D), C136(H13C,H13D), C64(H64A,H64B),
 C30(H30A,H30B)
3.d Aromatic/amide H refined with riding coordinates:
 C118(H118), C82(H82), C61(H61), C48(H48), C96(H96), C11(H11), C120(H120),
 C47(H47), C13(H13), C123(H123), C129(H129), C60(H60), C84(H84), C77(H77),
 C112(H112), C94(H94), C58(H58), C126(H126), C168(H168), C25(H25), C17(H17),
 C95(H95), C44(H44), C131(H131), C18(H18), C159(H159), C78(H78), C19(H19),
 C23(H23), C79(H79), C165(H165), C153(H153), C76(H76), C69(H69), C97(H97),
 C125(H125), C155(H155), C106(H106), C162(H162), C132(H132), C113(H113),
 C55(H55), C167(H167), C24(H24), C26(H26), C20(H20), C130(H130), C166(H166),
 C114(H114), C52(H52), C115(H115), C89(H89), C59(H59), C161(H161), C68(H68),
 C150(H150), C148(H148), C8(H8), C53(H53), C124(H124), C54(H54), C91(H91),
 C88(H88), C105(H105), C147(H147), C42(H42), C41(H41), C34(H34), C5(H5),
 C175(H175), C66(H66), C6(H6), C160(H160), C43(H43), C177(H177), C103(H103),
 C35(H35), C33(H33), C90(H90), C149(H149), C32(H32), C176(H176), C139(H139),
 C104(H104), C67(H67), C7(H7), C141(H141), C138(H138), C174(H174), C140(H140)
;