Two novel μ6-O2- bridged Co14/Ni14 hydroxamate Clusters packed in distorted face-centered cubic patterns
Zhang, Yanping; Lv, Rui; Wang, Jingyao; Yang, lin-yan; Liao, sheng-yun; Tian, Jin-Lei; Gu, Wen; Liu, Xin; Dalton Trans.  (2016) –; doi:10.1039/C5DT03974F

data_7038037
_publ_section_title
;
 Two novel \m6-O2- bridged Co14/Ni14 hydroxamate Clusters packed in
 distorted face-centered cubic patterns
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C5DT03974F
_journal_year                    2016
_chemical_formula_moiety         'C244 H220.55 Br28 N40 Ni28 O74'
_chemical_formula_sum            'C244 H220.54 Br28 N40 Ni28 O74'
_chemical_formula_weight         8778.49
_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   geom
_audit_creation_date             2016-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-15 deposited with the CCDC.
2016-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                83.25(3)
_cell_angle_beta                 72.87(3)
_cell_angle_gamma                64.81(3)
_cell_formula_units_Z            1
_cell_length_a                   17.868(4)
_cell_length_b                   20.685(4)
_cell_length_c                   29.557(6)
_cell_measurement_reflns_used    12731
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      25.9817
_cell_measurement_theta_min      1.6630
_cell_volume                     9446(4)
_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
;
????
;
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -110.0000 - 70.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 45.1341
              2theta: -19.9183
scan:
    Number of images: 150
               Slice: -110.0000 - 40.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.1341
              2theta: -19.9183
scan:
    Number of images: 100
               Slice: -110.0000 - -10.0000
         Image width: 1.0000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 45.1341
              2theta: -19.9183
;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0451
_diffrn_orient_matrix_UB_12      -0.0304
_diffrn_orient_matrix_UB_13      0.0342
_diffrn_orient_matrix_UB_21      -0.0173
_diffrn_orient_matrix_UB_22      0.0199
_diffrn_orient_matrix_UB_23      -0.0465
_diffrn_orient_matrix_UB_31      0.0174
_diffrn_orient_matrix_UB_32      -0.0253
_diffrn_orient_matrix_UB_33      -0.0176
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.1446
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            83882
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.034
_diffrn_reflns_theta_min         1.657
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    4.384
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4321
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.372
_refine_diff_density_min         -1.605
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1918
_refine_ls_number_reflns         36795
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1736
_refine_ls_R_factor_gt           0.0922
_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^)+(0.1415P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2393
_refine_ls_wR_factor_ref         0.2934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17389
_reflns_number_total             36795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03974f2.cif
_cod_data_source_block           ni14_sq
_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_original_cell_volume        9447(4)
_cod_database_code               7038037
_diffrn_number_total             36795
_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
 C118-N20
 1.39 with sigma of 0.01
 Br9A-C96A \\sim Br9-C96
 with sigma of 0.01
 Br9-C95 \\sim Br9-C95A
 with sigma of 0.01
3. Restrained planarity
 C96A, C97A, C98A, C93A, C94A, C95A, Br9A
 with sigma of 0.01
 Br9, C96, C97, C98, C93, C94, C95
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C92 \\sim C93 \\sim C98 \\sim C96 \\sim C97 \\sim C95 \\sim C94: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C93 \\sim C98 \\sim C97 \\sim C96 \\sim C95 \\sim C94 \\sim C97A \\sim C98A
\\sim C93A \\sim C94A \\sim C95A \\sim C96A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Br9 \\sim C95 \\sim C96 \\sim C97 \\sim C98: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C119) \\sim Ueq, Uanis(C118) \\sim Ueq, Uanis(C104) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C117) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C105) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br9A) \\sim Ueq, Uanis(Br9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(C98)=Sof(H98)=Sof(C97)=Sof(H97)=Sof(C96)=Sof(C95)=Sof(H95)=Sof(C94)=
 Sof(H94)=Sof(C93)=Sof(Br9)=1-FVAR(1)
 Sof(Br9A)=Sof(C97A)=Sof(C98A)=Sof(H98A)=Sof(C93A)=Sof(C94A)=Sof(H94A)=
 Sof(C95A)=Sof(H95A)=Sof(C96A)=FVAR(1)
6.a Me refined with riding coordinates:
 C103(H10P,H10Q,H10R), C104(H10S,H10T,H10U)
6.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C62(H62), C21(H21), C3(H3), C13(H13), C42(H42), C77(H77), C11(H11),
 C38(H38), C74(H74), C28(H28), C24(H24), C25(H25), C17(H17), C32(H32), C48(H48),
  C18(H18), C76(H76), C41(H41), C39(H39), C59(H59), C31(H31), C81(H81),
 C63(H63), C88(H88), C27(H27), C10(H10), C45(H45), C20(H20), C4(H4), C91(H91),
 C7(H7), C73(H73), C60(H60), C49(H49), C34(H34), C87(H87), C6(H6), C90(H90),
 C14(H14), C80(H80), C83(H83), C46(H46), C111(H111), C70(H70), C99(H99),
 C84(H84), C98(H98), C97(H97), C95(H95), C94(H94), C102(H102), C52(H52),
 C56(H56), C66(H66), C120(H120), C67(H67), C108(H108), C69(H69), C55(H55),
 C114(H114), C53(H53), C105(H105), C98A(H98A), C94A(H94A), C95A(H95A)
6.c Fitted hexagon refined as free rotating group:
 C98(C97,C96,C95,C94,C93), C97A(C98A,C93A,C94A,C95A,C96A)
6.d Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C), C113(H11A,H11B,H11C), C112(H11D,H11E,H11F), C122(H12A,
 H12B,H12C), C109(H10D,H10E,H10F), C121(H12D,H12E,H12F), C116(H11G,H11H,H11I),
 C110(H11J,H11K,H11L), C100(H10G,H10H,H10I), C106(H10J,H10K,H10L), C115(H11M,
 H11N,H11O), C107(H10M,H10N,H10O), C119(H11P,H11Q,H11R), C118(H11S,H11T,H11U)
;
_shelx_res_checksum              97302
_shelx_fab_checksum              7074
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'