Highly efficient structurally characterised novel precatalysts: di- and mononuclear heteroleptic Cu(i) dixanthate/xanthate‒phosphine complexes for azide‒alkyne cycloadditions
Anamika, Anamika; Agrahari, Anand K.; Manar, Krishna K.; Yadav, Chote Lal; Tiwari, Vinod K.; Drew, Michael G. B.; Singh, Nanhai; New Journal of Chemistry 43 (2019) 8939–; doi:10.1039/C9NJ01551E

data_7058364
_publ_section_title
;
 Highly efficient structurally characterised novel precatalysts: di- and
 mononuclear heteroleptic Cu(i) dixanthate/xanthate--phosphine complexes
 for azide--alkyne cycloadditions
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8939
_journal_paper_doi               10.1039/C9NJ01551E
_journal_volume                  43
_journal_year                    2019
_chemical_formula_sum            'C80.5 H73 Cl Cu2 O3 P4 S4'
_chemical_formula_weight         1503.03
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-02-04 deposited with the CCDC.    2019-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.427(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0078(10)
_cell_length_b                   15.7740(13)
_cell_length_c                   36.114(3)
_cell_measurement_reflns_used    111996
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.397
_cell_measurement_theta_min      2.030
_cell_volume                     7407.8(10)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker, Smart CCD Diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1315
_diffrn_reflns_av_unetI/netI     0.1277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            111910
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.397
_diffrn_reflns_theta_min         2.096
_exptl_absorpt_coefficient_mu    0.857
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       needle
_exptl_crystal_F_000             3116
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.735
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         18561
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1816
_refine_ls_R_factor_gt           0.0850
_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^)+(0.1265P)^2^+2.8580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2166
_refine_ls_wR_factor_ref         0.2439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9709
_reflns_number_total             18561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01551e2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7058360--7058364.cif.'
_cod_original_cell_volume        7407.7(10)
_cod_original_formula_sum        'C80.50 H73 Cl Cu2 O3 P4 S4'
_cod_database_code               7058364
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   1.000
_shelx_res_checksum              30247