Polynuclear Cu(i) and Ag(i) phosphine complexes containing multi-dentate polytopic ligands: syntheses, crystal structures and photoluminescence properties.
Xiang, Jing; Cheng, Shun-Cheung; Jin, Xin-Xin; Su, Qian-Qian; Zhou, Xin; Chu, Wing-Kin; Leung, Chi-Fai; Ko, Chi-Chiu; Dalton transactions (Cambridge, England : 2003) 48 (2019) 741–750; doi:10.1039/c8dt03377c

data_7048375
_publ_section_title
;
 Polynuclear Cu(i) and Ag(i) phosphine complexes containing multi-dentate
 polytopic ligands: syntheses, crystal structures and photoluminescence
 properties.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              741
_journal_page_last               750
_journal_paper_doi               10.1039/c8dt03377c
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_sum            'C86 H70 Ag2 B2 F8 N4 P4'
_chemical_formula_weight         1672.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-11-22 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.053(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.9776(8)
_cell_length_b                   10.6403(4)
_cell_length_c                   21.1006(9)
_cell_measurement_reflns_used    4287
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.6680
_cell_measurement_theta_min      4.2740
_cell_volume                     3947.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_unetI/netI     0.1349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28302
_diffrn_reflns_point_group_measured_fraction_full 0.872
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        67.224
_diffrn_reflns_theta_max         67.224
_diffrn_reflns_theta_min         2.513
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 1490 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(10)
_refine_ls_extinction_coef       0.00023(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     966
_refine_ls_number_reflns         12329
_refine_ls_number_restraints     2974
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0699
_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^)+(0.0506P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1801
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    0.744
_reflns_Friedel_fraction_max     0.744
_reflns_number_gt                6613
_reflns_number_total             12329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03377c2.cif
_cod_data_source_block           exp_7222
_cod_depositor_comments
'Adding full bibliography for 7048372--7048377.cif.'
_cod_database_code               7048375
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.677
_shelx_estimated_absorpt_t_max   0.708
_shelx_res_checksum              36006