A new strategy to obtain tetranuclear cobalt(ii) metal-organic frameworks based on the [Co4(μ3-OH)2] cluster: synthesis, structures and properties.
Li, Ke; Lv, Xiu-Xiu; Shi, Lu-Lu; Liu, Lu; Li, Bao-Long; Wu, Bing; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15078–15088; doi:10.1039/c6dt02895k

data_7040333
_publ_section_title
;
 A new strategy to obtain tetranuclear cobalt(ii) metal-organic frameworks
 based on the [Co4(\m3-OH)2] cluster: synthesis, structures and
 properties.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15078
_journal_page_last               15088
_journal_paper_doi               10.1039/c6dt02895k
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C36 H29 Co4 N9 O23'
_chemical_formula_sum            'C36 H29 Co4 N9 O23'
_chemical_formula_weight         1191.40
_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             2016-06-27
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-27 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                78.401(3)
_cell_angle_beta                 89.438(2)
_cell_angle_gamma                83.039(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7998(3)
_cell_length_b                   14.5731(5)
_cell_length_c                   17.0590(6)
_cell_measurement_reflns_used    9640
_cell_measurement_temperature    222.95(10)
_cell_measurement_theta_max      29.9130
_cell_measurement_theta_min      3.2560
_cell_volume                     2610.35(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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)'
_diffrn_ambient_temperature      222.95(10)
_diffrn_detector_area_resol_mean 10.4471
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -47.00   15.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6514  -77.0000  -60.0000 62

  2 omega   24.00   59.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       13.6514   37.0000 -150.0000 35

  3 omega    2.00   57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5889   37.0000   90.0000 55

  4 omega -105.00  -57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5889 -178.0000  -90.0000 48

  5 omega  -24.00   26.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5889  -99.0000 -120.0000 50

  6 omega  -25.00    0.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5889  -99.0000  -60.0000 25

  7 omega  -21.00   23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5889  -99.0000   60.0000 44

  8 omega  -92.00   19.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5889  -19.0000  120.0000 111
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0004163000
_diffrn_orient_matrix_UB_12      0.0339572000
_diffrn_orient_matrix_UB_13      0.0245525000
_diffrn_orient_matrix_UB_21      0.0175633000
_diffrn_orient_matrix_UB_22      -0.0365653000
_diffrn_orient_matrix_UB_23      0.0335890000
_diffrn_orient_matrix_UB_31      0.0637975000
_diffrn_orient_matrix_UB_32      0.0039687000
_diffrn_orient_matrix_UB_33      -0.0084279000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26543
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.599
_diffrn_reflns_theta_min         2.875
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          1
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         10935
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0497P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8732
_reflns_number_total             10935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02895k2.cif
_cod_data_source_block           2_sq
_cod_depositor_comments
;Adding full bibliography for 7040332--7040334.cif.

 Adding full bibliography for 7040332--7040334.cif.
;
_cod_original_cell_volume        2610.35(14)
_cod_database_code               7040333
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.349
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H10-O10
 0.9 with sigma of 0.001
 H7-O7
 0.9 with sigma of 0.001
3. Rigid bond restraints
 Co3, O4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(O17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O23A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: O16(0.75) O16A(0.25) O17(0.75) O17A(0.25) O18(0.5) O18A(0.3)
 O18B(0.2) O23(0.45) O23A(0.55)
6.a Rotating group:
 O19(H19A,H19B), O20(H20A,H20B), O21(H21A,H21B)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C10(H10A,H10B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15),
 C17(H17), C19(H19), C23(H23), C25(H25), C27(H27), C31(H31), C33(H33), C35(H35)
;
_shelx_res_checksum              61777
_shelx_fab_checksum              55043
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'