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_7129866
_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         'C20 H30 N4'
_chemical_formula_sum            'C20 H30 N4'
_chemical_formula_weight         326.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc29hh1c
_audit_creation_date             2021-03-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-20 deposited with the CCDC.	2022-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.287(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7820(3)
_cell_length_b                   9.2791(3)
_cell_length_c                   11.5020(5)
_cell_measurement_reflns_used    2227
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      66.7120
_cell_measurement_theta_min      5.0360
_cell_volume                     934.66(6)
_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      101(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4419
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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      0.1366199000
_diffrn_orient_matrix_UB_12      0.1038656000
_diffrn_orient_matrix_UB_13      -0.0029040000
_diffrn_orient_matrix_UB_21      0.0349886000
_diffrn_orient_matrix_UB_22      -0.0601553000
_diffrn_orient_matrix_UB_23      -0.1199312000
_diffrn_orient_matrix_UB_31      -0.1049027000
_diffrn_orient_matrix_UB_32      0.1147596000
_diffrn_orient_matrix_UB_33      -0.0605864000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8721
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.861
_diffrn_reflns_theta_max         66.861
_diffrn_reflns_theta_min         5.050
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015). Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0439P)^2^+0.2319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1302
_reflns_number_total             1655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00953f2.cif
_cod_data_source_block           ac_cb_c20h30n4_cu
_cod_database_code               7129866
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H30 N4'
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.910
_reflns_odcompleteness_completeness 97.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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:
 C5(H5), C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              27904
_olex2_date_sample_data_collection 2021-02-22
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_full_max 1.203
_oxdiff_exptl_absorpt_empirical_full_min 0.839