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_7711533
_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         'C53 H48 Cu N P4, 2(F6 P)'
_chemical_formula_sum            'C53 H48 Cu F12 N P6'
_chemical_formula_weight         1176.28
_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   geom
_audit_creation_date             2022-10-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-14 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.779(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7493(4)
_cell_length_b                   18.1851(4)
_cell_length_c                   13.2796(4)
_cell_measurement_reflns_used    43743
_cell_measurement_temperature    170
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.81
_cell_volume                     2554.97(14)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE & Cie, 2015)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE & Cie, 2016)'
_computing_data_reduction        'X-Area 1.90 (STOE & Cie, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.00
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22119
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.814
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.8281
_exptl_absorpt_correction_T_min  0.5964
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 3343 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(7)
_refine_ls_extinction_coef       0.026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         9055
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1231P)^2^+2.1389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.1864
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    0.804
_reflns_Friedel_fraction_max     0.797
_reflns_number_gt                8471
_reflns_number_total             9055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02338e2.cif
_cod_data_source_block           i2t2128_xshape
_cod_original_cell_volume        2554.97(13)
_cod_database_code               7711533
_shelx_shelxl_version_number     2019/2
_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
 P1A-F6A = P1A-F4A = P1A-F3A = P1A-F5A = P1A-F2A = P1A-F1A
 1.65 with sigma of 0.02
 F6A-F3A \\sim F4A-F5A \\sim F1A-F2A
 with sigma of 0.05
 P1A-F6A \\sim P1A-F4A \\sim P1A-F3A \\sim P1A-F5A \\sim P1A-F2A \\sim P1A-F1A
 with sigma of 0.02
 F6A-F4A \\sim F6A-F5A \\sim F6A-F2A \\sim F6A-F1A \\sim F3A-F4A \\sim F3A-F5A
\\sim F3A-F2A \\sim F3A-F1A
 with sigma of 0.04
 F6B-F5B \\sim F6B-F1B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
P1A \\sim F6A \\sim F4A \\sim F3A \\sim F5A \\sim F2A \\sim F1A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F6B \\sim F5B \\sim F1B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(F6A) = Uanis(F3A)
Uanis(F1A) = Uanis(F2A)
Uanis(F5A) = Uanis(F4A)
Uanis(F6B) = Uanis(F1A)
Uanis(F5A) = Uanis(F1B)
Uanis(F6A) = Uanis(F5B)
4. Rigid body (RIGU) restrains
 P1A, F6A, F4A, F3A, F5A, F2A, F1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F6B, F5B, F1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: F6A(0.5) F5A(0.5) F1A(0.5) F6B(0.5) F5B(0.5) F1B(0.5)
6.a Ternary CH refined with riding coordinates:
 C00N(H00N)
6.b Secondary CH2 refined with riding coordinates:
 C00H(H00A,H00B), C00T(H00C,H00D)
6.c Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M),
 C00O(H00O), C00Q(H00Q), C00R(H00R), C00S(H00S), C00U(H00U), C00V(H00V),
 C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C01A(H01A), C01B(H01B),
 C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01H(H01H), C01I(H01I),
 C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O),
 C01P(H01P), C01Q(H01Q), C01R(H01R), C011(H011), C012(H012), C013(H013),
 C015(H015), C016(H016), C018(H018), C019(H019)
6.d Idealised Me refined as rotating group:
 C01U(H01G,H01S,H01T)
;
_shelx_res_checksum              58002
_shelx_hkl_checksum              80318
_olex2_exptl_crystal_mounting_method 'glass fiber and Fomblin oil'
_olex2_submission_special_instructions 'No special instructions were received'