Two novel μ6-O2- bridged Co14/Ni14 hydroxamate Clusters packed in distorted face-centered cubic patterns
Zhang, Yanping; Lv, Rui; Wang, Jingyao; Yang, Linyan; Liao, Shengyun; Tian, Jinlei; Gu, Wen; Liu, Xin; Dalton Transactions 45 (2016) 3247–3250; doi:10.1039/C5DT03974F

data_7038038
_publ_section_title
;
 Two novel \m6-O2- bridged Co14/Ni14 hydroxamate Clusters packed in
 distorted face-centered cubic patterns
;
_journal_coden_ASTM              DTARAF
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              3247
_journal_page_last               3250
_journal_paper_doi               10.1039/C5DT03974F
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C121 H111 Br14 Co14 N20 O36, 8(C3 H7 N O)'
_chemical_formula_sum            'C145 H167 Br14 Co14 N28 O44'
_chemical_formula_weight         4949.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-11 deposited with the CCDC.
2016-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.020(4)
_cell_length_b                   30.995(6)
_cell_length_c                   31.396(6)
_cell_measurement_reflns_used    17900
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8784
_cell_measurement_theta_min      1.4137
_cell_volume                     18509(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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)'
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.1086
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            72315
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.896
_diffrn_reflns_theta_min         1.414
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    4.320
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.5227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       Prism
_exptl_crystal_F_000             9812
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.267
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Flack x determined using 4857 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1151
_refine_ls_number_reflns         21777
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+13.6265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1807
_reflns_Friedel_coverage         0.937
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                15751
_reflns_number_total             21777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03974f2.cif
_cod_data_source_block           co14_sq_s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               7038038
_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. Restrained distances
 N9-C54
 1.39 with sigma of 0.01
 N10-C60A = N10-C60
 1.45 with sigma of 0.01
 N11-C61 = N11-C61A
 1.3 with sigma of 0.01
 C67-H67
 1.39 with sigma of 0.01
3. Rigid bond restraints
 N10, C60A, C60, C59
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N11
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C40, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C71 \\sim C73 \\sim N15 \\sim C72 \\sim O24: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N11: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N11: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N11 \\sim C61 \\sim C61A: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(Br5) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(Br5A)=1-FVAR(1)
 Sof(Br5)=FVAR(1)
 Sof(C61)=Sof(H61D)=Sof(H61E)=Sof(H61F)=1-FVAR(2)
 Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(2)
 Fixed Sof: C60A(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C59(0.5) H59(0.5) C60(0.5)
 H60D(0.5) H60E(0.5) H60F(0.5)
6.a Me refined with riding coordinates:
 C65(H65A,H65B,H65C), C73(H73A,H73B,H73C), C71(H71A,H71B,H71C), C60A(H60A,H60B,
 H60C), C60(H60D,H60E,H60F), C61A(H61A,H61B,H61C), C61(H61D,H61E,H61F)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C21(H21), C28(H28), C20(H20), C3(H3), C6(H6), C17(H17), C14(H14),
 C18(H18), C31(H31), C4(H4), C35(H35), C13(H13), C46(H46), C25(H25), C27(H27),
 C45(H45), C32(H32), C48(H48), C34(H34), C49(H49), C7(H7), C24(H24), C11(H11),
 C42(H42), C41(H41), C38(H38), C56(H56), C50(H50), C53(H53), C39(H39), C67(H67),
  C64(H64), C69(H69), C72(H72), C59(H59)
6.c Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C57(H57A,H57B,H57C), C52(H52A,H52B,H52C), C55(H55A,H55B,
 H55C), C54(H54A,H54B,H54C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C), C68(H68A,
 H68B,H68C), C70(H70A,H70B,H70C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              97690
_shelx_fab_checksum              4093
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'