Synthesis and Disassembly of an Organometallic Polymer Comprising Redox-active Co4S4 Clusters and Janus Biscarbene Linkers
Gillen , Jonathan; Moore, Connor; Vuong, My; Shajahan, Juvairia; Anstey, Mitchell Ryan; Alston, Jeffrey R.; Bejger, Christopher Michael; Chemical Communications  (2022) –; doi:10.1039/D2CC00953F

data_7129865
_publ_section_title
;
 Synthesis and Disassembly of an Organometallic Polymer Comprising
 Redox-active Co4S4 Clusters and Janus Biscarbene Linkers
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00953F
_journal_year                    2022
_chemical_formula_moiety         'C52 H72 Co4 N8 S4'
_chemical_formula_sum            'C52 H72 Co4 N8 S4'
_chemical_formula_weight         1173.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc29hh0b
_audit_creation_date             2020-12-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-12-20 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                94.342(3)
_cell_angle_beta                 95.063(3)
_cell_angle_gamma                93.514(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9073(5)
_cell_length_b                   13.2862(5)
_cell_length_c                   17.5673(6)
_cell_measurement_reflns_used    13965
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.2120
_cell_measurement_theta_min      3.6450
_cell_volume                     2985.22(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4419
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.900
_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    -82.00  19.00   1.00    4.09    --   -8.98 -57.00   0.00  101
  2  \w    -19.00  82.00   1.00    4.09    --    9.13  57.00 -90.00  101
  3  \w     -4.00  50.00   1.00    4.09    --    9.13 -99.00  30.00   54
  4  \w    -23.00  85.00   1.00    4.09    --    9.13  77.00 -90.00  108
  5  \w    -67.00  42.00   1.00    4.09    --    9.13 -77.00 150.00  109
  6  \w    -15.00  83.00   1.00    4.09    --    9.13  38.00-180.00   98
  7  \w     -4.00  50.00   1.00    4.09    --    9.13 -99.00  60.00   54
  8  \w     -4.00  50.00   1.00    4.09    --    9.13 -99.00-150.00   54
  9  \w     -4.00  25.00   1.00    4.09    --    9.13 -99.00   0.00   29
 10  \w     -4.00  50.00   1.00    4.09    --    9.13 -99.00 -90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0356113000
_diffrn_orient_matrix_UB_12      0.0367241000
_diffrn_orient_matrix_UB_13      -0.0124031000
_diffrn_orient_matrix_UB_21      -0.0420331000
_diffrn_orient_matrix_UB_22      0.0226455000
_diffrn_orient_matrix_UB_23      -0.0193269000
_diffrn_orient_matrix_UB_31      -0.0047893000
_diffrn_orient_matrix_UB_32      0.0319148000
_diffrn_orient_matrix_UB_33      0.0335661000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59734
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.632
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.481
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         13795
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0321P)^2^+2.7770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10150
_reflns_number_total             13795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00953f2.cif
_cod_data_source_block           g2-50
_cod_database_code               7129865
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co4 S4 N8 C52 H72'
_chemical_oxdiff_usercomment     JG_CB_Co4S4N8C52H72
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.580
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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.a Ternary CH refined with riding coordinates:
 C24(H24), C21(H21), C47(H47), C50(H50), C37(H37), C34(H34), C8(H8), C11(H11)
2.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C44(H44), C19(H19), C46(H46), C18(H18), C20(H20), C17(H17),
 C45(H45), C33(H33), C30(H30), C7(H7), C32(H32), C31(H31), C6(H6), C4(H4),
 C5(H5)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C51(H51A,H51B,
 H51C), C38(H38A,H38B,H38C), C49(H49A,H49B,H49C), C22(H22A,H22B,H22C), C25(H25A,
 H25B,H25C), C23(H23A,H23B,H23C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C),
 C35(H35A,H35B,H35C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C13(H13A,H13B,
 H13C), C9(H9A,H9B,H9C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 45 electrons were 
found in a volume of 445\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.5[C4H10O] per Asymmetric Unit 
which account for 42 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2370
_shelx_fab_checksum              80582
_olex2_date_sample_data_collection 2020-12-17
_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 1.180
_oxdiff_exptl_absorpt_empirical_full_min 0.876