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_7711530
_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_absolute_configuration unk
_chemical_formula_moiety         'C51 H45 Ag Br P4, F6 P, 0.75(C4 H10 O)'
_chemical_formula_sum            'C54 H52.5 Ag Br F6 O0.75 P5'
_chemical_formula_weight         1170.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-09-06
_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                 115.34(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.695(2)
_cell_length_b                   18.914(4)
_cell_length_c                   13.280(3)
_cell_measurement_reflns_used    416
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      26.52
_cell_measurement_theta_min      5.09
_cell_volume                     2654.9(11)
_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)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19821
_diffrn_reflns_point_group_measured_fraction_full 0.820
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.173
_diffrn_reflns_theta_min         2.742
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  0.7974
_exptl_absorpt_correction_T_min  0.5560
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED 32 Version 1.57, 2011 STOE & Cie GmbH'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       plate
_exptl_crystal_F_000             1187
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.113
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.020(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         11400
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0748P)^2^+0.8454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.561
_reflns_Friedel_fraction_full    0.633
_reflns_Friedel_fraction_max     0.589
_reflns_number_gt                10115
_reflns_number_total             11400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02338e2.cif
_cod_data_source_block           p21
_cod_original_formula_sum        'C54 H52.50 Ag Br F6 O0.75 P5'
_cod_database_code               7711530
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.609
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H74-C74
 0.95 with sigma of 0.02
 P3-H74 \\sim P5-H74
 with sigma of 0.02
3. Others
 Fixed Sof: O10(0.75) C15(0.75) H15A(0.75) H15B(0.75) C16(0.75) H16A(0.75)
 H16B(0.75) H16C(0.75) C26(0.75) H26A(0.75) H26B(0.75) C27(0.75) H27A(0.75)
 H27B(0.75) H27C(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C60(H60A,H60B), C15(H15A,H15B), C26(H26A,H26B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13),
 C14(H14), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C29(H29), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36),
 C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C44(H44), C47(H47), C51(H51),
  C53(H53), C57(H57), C58(H58), C59(H59), C61(H61), C63(H63), C67(H67), C68(H68)
4.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              88618
_shelx_hkl_checksum              74435
_olex2_submission_special_instructions 'No special instructions were received'