Luminescent Triphosphine Cyanide d(10) Metal Complexes.
Chakkaradhari, Gomathy; Chen, Yi-Ting; Karttunen, Antti J.; Dau, Minh Thuy; Jänis, Janne; Tunik, Sergey P.; Chou, Pi-Tai; Ho, Mei-Lin; Koshevoy, Igor O.; Inorganic chemistry 55 (2016) 2174–2184; doi:10.1021/acs.inorgchem.5b02581

data_4347008
_publ_section_title
;
 Luminescent Triphosphine Cyanide d(10) Metal Complexes.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2174
_journal_page_last               2184
_journal_paper_doi               10.1021/acs.inorgchem.5b02581
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'2(C85 H66 Cu2 N P6), 2(C F3 O3 S), 3(C H2 Cl2)'
_chemical_formula_sum            'C175 H138 Cl6 Cu4 F6 N2 O6 P12 S2'
_chemical_formula_weight         3381.49
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                105.562(4)
_cell_angle_beta                 107.131(4)
_cell_angle_gamma                112.836(3)
_cell_formula_units_Z            1
_cell_length_a                   17.0857(12)
_cell_length_b                   17.1852(12)
_cell_length_c                   17.312(2)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.63
_cell_measurement_theta_min      2.40
_cell_volume                     4032.4(7)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'Diamond v.3.2g (Brandenburg, 2011)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '62mm x 62mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II DUO CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'curved graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            81751
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.955
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             1734
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.271
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.449
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1923
_refine_ls_number_reflns         34389
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0745P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                29313
_reflns_number_total             34389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02581_si_003.cif
_cod_data_source_block           4a
_cod_original_cell_volume        4032.5(6)
_cod_database_code               4347008
_shelx_estimated_absorpt_t_min   0.804
_shelx_estimated_absorpt_t_max   0.820
_shelxl_version_number           2014/6
_shelx_res_checksum              13735
_shelx_hkl_checksum              70535