Synthesis of the first chiral polynuclear copper(i) complex based on (R)-1-(1-phenyl)ethyl-3-(O,O-diethylthiophosphoryl)thiourea and its characterization in the solid state and solution
Metlushka, Kirill E.; Sadkova, Dilyara N.; Nikitina, Kristina A.; Pashagin, Alexander V.; Khrizanforov, Mikhail N.; Budnikova, Yulia H.; Morozov, Vladimir I.; Islamov, Daut R.; Latypov, Shamil K.; Kataeva, Olga N.; Alfonsov, Vladimir A.; New Journal of Chemistry 44 (2020) 3224–3231; doi:10.1039/C9NJ05683A

data_7059356
_publ_section_title
;
 Synthesis of the first chiral polynuclear copper(i) complex based on
 (R)-1-(1-phenyl)ethyl-3-(O,O-diethylthiophosphoryl)thiourea and its
 characterization in the solid state and solution
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3224
_journal_page_last               3231
_journal_paper_doi               10.1039/C9NJ05683A
_journal_volume                  44
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C78 H120 Cu6 N12 O12 P6 S12, C H4 O'
_chemical_formula_sum            'C79 H124 Cu6 N12 O13 P6 S12'
_chemical_formula_weight         2401.67
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-01-04 deposited with the CCDC.	2020-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.9271(9)
_cell_length_b                   13.5236(7)
_cell_length_c                   22.1821(11)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.53
_cell_volume                     5312.3(5)
_computing_cell_refinement       'APEX3 v2018.7-2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT NT v6.0 (Bruker AXS, 2003)'
_computing_molecular_graphics    'Mercury CSD 4.1.0'
_computing_publication_material  'enCIFer Version 1.7.1'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker Kappa Apex DUO'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            236246
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.770
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.160
_refine_diff_density_max         2.158
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 8599 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1203
_refine_ls_number_reflns         20886
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+9.8617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                19318
_reflns_number_total             20886
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj05683a2.cif
_cod_data_source_block           kar94
_cod_depositor_comments          'Adding full bibliography for 7059356.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7059356
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.690
_shelx_estimated_absorpt_t_max   0.788
_shelx_res_checksum              25393