Bis(diphenylphosphinyl)-functionalized dipyrido-annulated NHC towards copper(i) and silver(i).
Zhang, Sihan; Shang, Rong; Nakamoto, Masaaki; Yamamoto, Yohsuke; Adachi, Yohei; Ohshita, Joji; Dalton transactions (Cambridge, England : 2003) 48 (2019) 12250–12256; doi:10.1039/c9dt02435b

data_7700493
_publ_section_title
;
 Bis(diphenylphosphinyl)-functionalized dipyrido-annulated NHC towards
 copper(i) and silver(i).
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12250
_journal_page_last               12256
_journal_paper_doi               10.1039/c9dt02435b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C43 H42 Br4 Cu4 N2 P2'
_chemical_formula_weight         1222.52
_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-2014/5
_audit_update_record
;
2019-06-01 deposited with the CCDC.    2019-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.0900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3808(6)
_cell_length_b                   25.6046(17)
_cell_length_c                   18.5364(12)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.71
_cell_measurement_theta_min      2.33
_cell_volume                     4418.2(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1118
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23849
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.726
_diffrn_reflns_theta_min         1.938
_exptl_absorpt_coefficient_mu    5.622
_exptl_absorpt_correction_T_max  0.399
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.637
_refine_diff_density_min         -1.535
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         9337
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+8.6060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7255
_reflns_number_total             9337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02435b2.cif
_cod_data_source_block           6_Cu4LBr4
_cod_depositor_comments
;
Adding full bibliography for 7700491--7700494.cif.

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C86 H84 Br8 Cu8 N4 P4'
_cod_original_formula_weight         2445.05
_cod_original_formula_units_Z            2
_cod_database_code               7700493
_shelx_estimated_absorpt_t_max   0.399
_shelx_estimated_absorpt_t_min   0.165
_shelxl_version_number           2014/5
_shelx_res_checksum              13181