Supramolecular chirality in the crystals of mononuclear and polymeric cobalt(ii) complexes with enantiopure and racemic N-thiophosphorylated thioureas
Kataeva, Olga; Metlushka, Kirill; Ivshin, Kamil; Yamaleeva, Zilya; Zinnatullin, Ruzal; Nikitina, Kristina; Badeeva, Elena; Khrizanforova, Vera; Budnikova, Yulia; Naumann, Marco; Wellm, Christoph; Alfonsov, Alexey; Kataev, Vladislav; Büchner, Bernd; Knupfer, Martin; CrystEngComm 23 (2021) 2081–2090; doi:10.1039/D0CE01871F

data_7242167
_publ_section_title
;
 Supramolecular chirality in the crystals of mononuclear and polymeric
 cobalt(ii) complexes with enantiopure and racemic N-thiophosphorylated
 thioureas
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2081
_journal_page_last               2090
_journal_paper_doi               10.1039/D0CE01871F
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C31 H45 Co N5 O4 P2 S4'
_chemical_formula_sum            'C31 H45 Co N5 O4 P2 S4'
_chemical_formula_weight         800.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-12-20 deposited with the CCDC.	2021-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.75(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.632(7)
_cell_length_b                   19.326(19)
_cell_length_c                   12.434(8)
_cell_measurement_reflns_used    134
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      12.73
_cell_measurement_theta_min      2.38
_cell_volume                     2055(3)
_computing_cell_refinement       'APEX3 v2018.1-0'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT NT v6.0 (Bruker AXS, 2003)'
_computing_molecular_graphics    'Mercury 2020.1'
_computing_publication_material  'enCIFer 2020.1'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.1333
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17748
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.107
_diffrn_reflns_theta_min         1.960
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.7351
_exptl_absorpt_correction_T_min  0.5025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1064 before and 0.0697 after correction.
The Ratio of minimum to maximum transmission is 0.6836.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       prism
_exptl_crystal_F_000             838
_exptl_crystal_size_max          0.789
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 1918 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         9275
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0785P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.883
_reflns_number_gt                5831
_reflns_number_total             9275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01871f2.cif
_cod_data_source_block           k8_27
_cod_depositor_comments
'Adding full bibliography for 7242167--7242170.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7242167
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.594
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              70715