Two Triazole-Based Phosphine Ligands Prepared via Temperature-Mediated Li/H Exchange: Cu(I) and Au(I) Complexes and Structural Studies.
Choubey, Bimba; Radhakrishna, Latchupatula; Mague, Joel T.; Balakrishna, Maravanji S.; Inorganic chemistry 55 (2016) 8514–8526; doi:10.1021/acs.inorgchem.6b01094

data_4348274
_publ_section_title
;
 Two Triazole-Based Phosphine Ligands Prepared via Temperature-Mediated
 Li/H Exchange: Cu(I) and Au(I) Complexes and Structural Studies.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8514
_journal_page_last               8526
_journal_paper_doi               10.1021/acs.inorgchem.6b01094
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C54 H45 Cu2 N7 O P2, 2(B F4), C H2 Cl2'
_chemical_formula_sum            'C55 H47 B2 Cl2 Cu2 F8 N7 O P2'
_chemical_formula_weight         1255.53
_chemical_name_systematic
;
{\m-(1-[2-diphenylphosphanyl)phenyl]-4-phenyl-1H-1,2,3-triazole-
1\k^2^<i>P,N</i>; 2\k<i>N</i>}{\m-(1-[2-diphenylphosphanyl)phenyl]-
4-phenyl-1H-1,2,3-triazole-1\k<i>N</i>; 2\k^2^<i>P,N</i>}(aqua-
1\k<i>O</i>)(acetonitrile-2\k<i>N</i>)dicopper(I) tetrafluoroborate 
dichloromethane solvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                100.6880(10)
_cell_angle_beta                 92.7270(11)
_cell_angle_gamma                107.2020(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2654(7)
_cell_length_b                   12.6027(9)
_cell_length_c                   22.9535(16)
_cell_measurement_reflns_used    9561
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.7002
_cell_measurement_theta_min      2.2616
_cell_volume                     2770.8(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3660
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25873
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         28.713
_diffrn_reflns_theta_min         1.778
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>TWINABS</i> (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_transmission_factor_max   0.942
_exptl_transmission_factor_min   0.632
_refine_diff_density_max         1.485
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         13923
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0590P)^2^+1.0739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10199
_reflns_number_total             13923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01094_si_005.cif
_cod_data_source_block           msb651_a
_cod_database_code               4348274
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.952
_shelxl_version_number           2013-3
_shelx_res_checksum              83021
_shelx_hkl_checksum              21714