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_7711539
_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 Cl Cu P4, F6 P, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C52.5 H48 Cl4 Cu F6 P5'
_chemical_formula_weight         1153.10
_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             2019-01-16
_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                 105.7150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.7110(10)
_cell_length_b                   11.7151(5)
_cell_length_c                   38.1889(19)
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.362
_cell_volume                     10211.5(8)
_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)'
_diffrn_ambient_temperature      99.99
_diffrn_detector                 'Photon 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CMOS active pixel sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0989
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            62444
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.427
_diffrn_reflns_theta_min         2.124
_diffrn_source                   'I\mS Microfocus Source'
_diffrn_source_type              'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_T_max  0.0932
_exptl_absorpt_correction_T_min  0.0691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0945 before and 0.0599 after correction. The Ratio of minimum to maximum transmission is 0.7414. 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    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             4712
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         10472
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+31.0681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7472
_reflns_number_total             10472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02338e2.cif
_cod_data_source_block           lmcdp259_0ma_neu_a
_cod_original_formula_sum        'C52.50 H48 Cl4 Cu F6 P5'
_cod_database_code               7711539
_shelx_shelxl_version_number     2014/7
_audit_contact_author            'L. Maser'
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.920
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl10-C1 \\sim Cl-C1
 with sigma of 0.02
3. Others
 Fixed Sof: Cl10(0.5) C1(0.5) H1A(0.5) H1B(0.5) Cl(0.5)
4.a Ternary CH refined with riding coordinates:
 C00R(H00R)
4.b Secondary CH2 refined with riding coordinates:
 C00L(H00A,H00B), C00M(H00C,H00D), C01W(H01W,H01X), C1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C017(H017), C018(H018), C019(H019),
 C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F),
 C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V)
;
_olex2_submission_special_instructions 'No special instructions were received'