The dominance of sulfate over two organic ligands in the solvothermal assembly of an undecanuclear cobaltous cluster: crystallography and mass spectrometry.
Jiang, Li-Ping; Kurmoo, Mohamedally; Zeng, Ming-Hua; Dalton transactions (Cambridge, England : 2003) 49 (2020) 17683–17688; doi:10.1039/d0dt02880k

data_7705756
_publ_section_title
;
 The dominance of sulfate over two organic ligands in the solvothermal
 assembly of an undecanuclear cobaltous cluster: crystallography and mass
 spectrometry.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17683
_journal_page_last               17688
_journal_paper_doi               10.1039/d0dt02880k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'C72 H104 Co11 N16 O50 S8, 2(C0.5 H2.5 O0.5), 5(C H4 O)'
_chemical_formula_sum            'C78 H129 Co11 N16 O56 S8'
_chemical_formula_weight         3091.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-10 deposited with the CCDC.	2020-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.282(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.5656(12)
_cell_length_b                   20.2178(6)
_cell_length_c                   27.3542(13)
_cell_measurement_reflns_used    10582
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9240
_cell_measurement_theta_min      2.9270
_cell_volume                     11849.8(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -64.00 -37.00   0.50    5.00    --  -43.80  92.00  -6.00   54
  2  \w    -16.00  28.00   0.50    5.00    --  -43.80  92.00  -6.00   88
  3  \w    -81.00 -23.00   0.50   20.00    --  -90.25 125.00  90.00  116
  4  \w    -96.00 -71.00   0.50   20.00    --  -90.25  92.00  -6.00   50
  5  \w   -118.00 -21.00   0.50    5.00    --  -43.80 -57.00-120.00  194
  6  \w     47.00  75.00   0.50    5.00    --   43.80 -92.00-118.00   56
  7  \w     41.00 134.00   0.50   20.00    --  111.75 -45.00-120.00  186
  8  \w     81.00 131.00   0.50   20.00    --  111.75 -92.00-118.00  100
  9  \w     41.00 104.00   0.50   20.00    --  111.75 -94.00-180.00  126
 10  \w     -3.00  79.00   0.50    5.00    --   43.80 -99.00  60.00  164
 11  \w     38.00  65.00   0.50   20.00    --  111.75 -94.00 120.00   54
 12  \w     39.00 106.00   0.50   20.00    --  111.75 -94.00  60.00  134
 13  \w     41.00  91.00   0.50   20.00    --  111.75 -94.00 150.00  100
 14  \w    -21.00  43.00   0.50    5.00    --   43.80 -92.00-118.00  128
 15  \w    -73.00 -44.00   0.50    5.00    --  -43.80-178.00  30.00   58
 16  \w   -152.00-119.00   0.50   20.00    --  -90.25 -92.00-118.00   66
 17  \w     99.00 178.00   0.50   20.00    --  111.75  92.00  -6.00  158
 18  \w    152.00 178.00   0.50   20.00    --  111.75 125.00   0.00   52
 19  \w    102.00 128.00   0.50   20.00    --  111.75 125.00   0.00   52
 20  \w     93.00 134.00   0.50   20.00    --  111.75 125.00 -60.00   82
 21  \w    107.00 162.00   0.50   20.00    --  111.75  77.00 -60.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0652216000
_diffrn_orient_matrix_UB_12      0.0316365000
_diffrn_orient_matrix_UB_13      -0.0315017000
_diffrn_orient_matrix_UB_21      -0.0253022000
_diffrn_orient_matrix_UB_22      -0.0625486000
_diffrn_orient_matrix_UB_23      -0.0365417000
_diffrn_orient_matrix_UB_31      -0.0164535000
_diffrn_orient_matrix_UB_32      -0.0297785000
_diffrn_orient_matrix_UB_33      0.0430066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34206
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.064
_diffrn_reflns_theta_max         67.064
_diffrn_reflns_theta_min         2.954
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.909
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       block
_exptl_crystal_F_000             6328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.321
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         10554
_refine_ls_number_restraints     412
_refine_ls_restrained_S_all      2.539
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1501P)^2^+42.7212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2256
_refine_ls_wR_factor_ref         0.2429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8120
_reflns_number_total             10554
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02880k2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7705756.cif.'
_cod_database_code               7705756
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Co C H O N Cl'
_shelx_estimated_absorpt_t_max   0.337
_shelx_estimated_absorpt_t_min   0.167
_reflns_odcompleteness_completeness 99.79
_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
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Restrained distances
 C34-O23 = C35-O24 = C36-O25
 1.419 with sigma of 0.001
 O31_$1-C41_$1 = C38_$2-O27_$2
 1.419 with sigma of 0.001
 C37-O26
 1.419 with sigma of 0.001
 O23-H23
 0.96 with sigma of 0.001
 C40-O29 = C39-O28
 1.419 with sigma of 0.01
 O20-H20A
 0.86 with sigma of 0.02
 O20-H20B
 0.86 with sigma of 0.02
 O22-H22B
 0.86 with sigma of 0.02
 O22-H22A
 0.86 with sigma of 0.02
 O25-H25
 0.86 with sigma of 0.02
 H24-O24
 0.86 with sigma of 0.02
 C41-O31
 1.41 with sigma of 0.02
 C41-O30
 1.41 with sigma of 0.02
 O26-H26A
 0.86 with sigma of 0.02
 N8-H8B
 1.035 with sigma of 0.001
 N8-H8A
 1.035 with sigma of 0.001
 H8B-H8A
 1.646 with sigma of 0.001
3. Rigid bond restraints
 O23, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C34) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) = Uanis(O25)
Uanis(C35) = Uanis(O24)
Uanis(C6) = Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C4) = Uanis(C5)
Uanis(C34) = Uanis(O23)
Uiso(O26) = Uiso(C37)
Uiso(O31) = Uiso(C41)
Uiso(C41) = Uiso(O31)
Uiso(O28) = Uiso(C39)
Uiso(O29) = Uiso(C40)
Uanis(C18) = Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17)
Uiso(O31) = Uiso(C41) = Uiso(O30)
5. Rigid body (RIGU) restrains
 O1, N1, N2, C1, C2, C3, C4, C5, C6, C7, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, N3, N4, C10, C11, C12, C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N7, N8, C28, C29, C30, C31, C32, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, N5, N6, C19, C20, C21, C22, C23, C24, C25, C26, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O26(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) O27(0.5) H27(0.5)
 C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) O28(0.5) H28(0.5) C39(0.5) H39A(0.5)
 H39B(0.5) H39C(0.5) O29(0.5) H29(0.5) C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5)
 O30(0.5) H30A(0.5) O31(0.5) H31A(0.5) H41A(0.5) H41B(0.5) H41C(0.5) H41D(0.5)
 H41E(0.5) H41F(0.5)
7.a Riding coordinates:
 O20(H20A,H20B), O21(H21A,H21B), O22(H22A,H22B), O23(H23), O24(H24), O25(H25),
 N8(H8A,H8B), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), O27(H27), C38(H38A,H38B,H38C), O28(H28), C39(H39A,H39B,
 H39C), O29(H29), C40(H40A,H40B,H40C), O30(H30A), O31(H31A), C41(H41A,H41B,
 H41C), C41(H41D,H41E,H41F)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C10(H10A,H10B), C19(H19A,H19B), C28(H28A,H28B)
7.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17),
 C23(H23A), C25(H25A), C26(H26), C30(H30), C31(H31), C32(H32), C33(H33)
7.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C12(H12A,H12B,H12C), C21(H21C,H21D,H21E)
;
_shelx_res_checksum              46357
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.544
_oxdiff_exptl_absorpt_empirical_full_min 0.499
_publcif_funding_html
;
;