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_7711537
_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         'C53 H48 Ag N P4, 2(F6 P)'
_chemical_formula_sum            'C53 H48 Ag F12 N P6'
_chemical_formula_weight         1220.61
_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
_audit_creation_date             2021-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-12 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.4520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6318(5)
_cell_length_b                   18.2132(7)
_cell_length_c                   13.3823(6)
_cell_measurement_reflns_used    9384
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.25
_cell_volume                     2559.92(19)
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v3.0.26'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Photon 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CMOS active pixel sensor'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'fixed-chi goniometer'
_diffrn_measurement_device_type  'D8 Quest (Bruker AXS Inc.)'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            86094
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_min         2.236
_diffrn_source                   'I\mS Microfocus Source'
_diffrn_source_type              'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.0242
_exptl_absorpt_correction_T_min  0.0060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1300 before and 0.0556 after correction. The Ratio of minimum to maximum transmission is 0.2479. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.328
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 5033 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         11908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0581P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.894
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                11277
_reflns_number_total             11908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02338e2.cif
_cod_data_source_block           lmcdp251a_0m_biggermu_a
_cod_original_cell_volume        2559.91(19)
_cod_database_code               7711537
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'L. Maser'
_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.a Secondary CH2 refined with riding coordinates:
 C00S(H00A,H00B), C017(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00L(H00L), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00T(H00T), C00U(H00U), C00V(H00V), C00X(H00X), C00Z(H00Z),
 C011(H011), C012(H012), C013(H013), C014(H014), C015(H015), C018(H018),
 C019(H019), C01A(H01C), C01B(H01D), C01C(H01E), C01D(H01F), C01E(H01G),
 C01F(H01H), C01H(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M),
 C01N(H01N), C01Q(H01Q), C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V),
 C01W(H01W), C01X(H01X), C01Y(H01Y), C01Z(H01Z)
2.c Idealised Me refined as rotating group:
 C021(H02A,H02B,H02C)
;
_shelx_res_checksum              20280
_shelx_hkl_checksum              39809
_olex2_submission_special_instructions 'No special instructions were received'