Cationic ligands between σ-donation and hydrogen-bridge-bond- stabilisation of ancillary ligands in coinage metal complexes with protonated carbodiphosphoranes
Maser, Leon; Vogt, Matthias; Langer, Robert; Dalton Transactions  (2022) –; doi:10.1039/D2DT02338E

data_7711532
_publ_section_title
;
 Cationic ligands between \s-donation and hydrogen-bridge-bond-
 stabilisation of ancillary ligands in coinage metal complexes with
 protonated carbodiphosphoranes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02338E
_journal_year                    2022
_chemical_formula_moiety         'C51 H45 Br Cu P4, F6 P, 1.394(C H2 Cl2)'
_chemical_formula_sum            'C52.39 H47.79 Br Cl2.79 Cu F6 P5'
_chemical_formula_weight         1188.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-05-12 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.849(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.897(2)
_cell_length_b                   11.8212(7)
_cell_length_c                   38.426(3)
_cell_measurement_reflns_used    501
_cell_measurement_temperature    170.15
_cell_measurement_theta_max      25.335
_cell_measurement_theta_min      1.98
_cell_volume                     10442.4(14)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1688
_diffrn_reflns_av_unetI/netI     0.1031
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            47825
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.215
_diffrn_reflns_theta_min         2.699
_exptl_absorpt_coefficient_mu    1.537
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       plank
_exptl_crystal_F_000             4820
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         13794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0880
_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^)+(0.1070P)^2^+82.1918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2167
_refine_ls_wR_factor_ref         0.2577
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9272
_reflns_number_total             13794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02338e2.cif
_cod_data_source_block           i2t2122_pl
_cod_database_code               7711532
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.565
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl2) = Uanis(Cl4) = Uanis(C51)
3. Others
 Fixed Sof: Cl1(0.8936) Cl3(0.8936) C38(0.8936) H38A(0.8936) H38B(0.8936)
 Cl2(0.5) Cl4(0.5) C51(0.5) H51A(0.5) H51B(0.5)
4.a Ternary CH refined with riding coordinates:
 C9(H9)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C38(H38A,H38B), C51(H51A,H51B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34),
 C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
 C53(H53), C54(H54)
;
_shelx_res_checksum              8595
_shelx_hkl_checksum              85233
_olex2_submission_special_instructions 'No special instructions were received'