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_7058361
_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            'C81 H67 Cu2 N O2 P4 S4'
_chemical_formula_weight         1465.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                88.922(9)
_cell_angle_beta                 67.762(10)
_cell_angle_gamma                61.724(10)
_cell_formula_units_Z            1
_cell_length_a                   12.8039(13)
_cell_length_b                   12.9993(12)
_cell_length_c                   13.5744(15)
_cell_measurement_reflns_used    12833
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.20
_cell_volume                     1805.7(4)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL, PLATON, WINGX (Ferrugia, 2012)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.1368
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10789
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.604
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             758
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         8090
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1515
_refine_ls_R_factor_gt           0.0795
_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^)+(0.0648P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4338
_reflns_number_total             8090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01551e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7058360--7058364.cif.'
_cod_database_code               7058361
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              64940