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_7711531
_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 Cu I P4, F5.6 P0.9, 0.1(F4 P), 0.875[CH2Cl2], 0.5[CH2Cl2]'
_chemical_formula_sum            'C51 H45 Cu F6 I P5'
_chemical_formula_weight         1117.16
_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             2022-10-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-12 deposited with the CCDC.	2022-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.076(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.0323(14)
_cell_length_b                   11.9050(5)
_cell_length_c                   39.489(2)
_cell_measurement_reflns_used    54991
_cell_measurement_temperature    170
_cell_measurement_theta_max      29.72
_cell_measurement_theta_min      2.32
_cell_volume                     10611.5(10)
_computing_cell_refinement       'X-Area Recipe 1.36.0.0 (STOE, 2020)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area X-Red 1.65.2.0 (STOE, 2020)
;
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 215 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            41551
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.331
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           30
_diffrn_source_power             1.500
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  0.8243
_exptl_absorpt_correction_T_min  0.2531
_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            colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4496
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.272
_exptl_crystal_size_min          0.171
_refine_diff_density_max         0.707
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.00036(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         10434
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0555
_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^)+(0.1018P)^2^+34.2222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1754
_reflns_d_resolution_high        0.727
_reflns_d_resolution_low         8.728
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              32
_reflns_limit_h_min              -32
_reflns_limit_k_max              13
_reflns_limit_k_min              -16
_reflns_limit_l_max              54
_reflns_limit_l_min              -54
_reflns_number_gt                8948
_reflns_number_total             10434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02338e2.cif
_cod_data_source_block           i2t2123
_cod_original_cell_volume        10611.4(10)
_cod_database_code               7711531
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P2-F4 = P2-F6 = P2-F7 = P2-F8
 1.65 with sigma of 0.02
 F4-F6 \\sim F8-F7
 with sigma of 0.05
 P2-F4 \\sim P2-F6 \\sim P2-F7 \\sim P2-F8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P2 \\sim F4 \\sim F6 \\sim F7 \\sim F8: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 P2, F4, F6, F7, F8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: P007(0.9) F00A(0.9) F00H(0.9) F00K(0.9) F00X(0.9) P2(0.1) F4(0.1)
 F6(0.1) F7(0.1) F8(0.1)
6.a Ternary CH refined with riding coordinates:
 C00J(H00J)
6.b Secondary CH2 refined with riding coordinates:
 C00F(H00A,H00B), C00P(H00C,H00D)
6.c Aromatic/amide H refined with riding coordinates:
 C01G(H01G), C01R(H01R), C01T(H01T), C01U(H01U), C01S(H01S), C00O(H00O),
 C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
 C00W(H00W), C00Y(H00Y), C00Z(H00Z), C010(H010), C011(H011), C012(H012),
 C013(H013), C014(H014), C016(H016), C017(H017), C018(H018), C019(H019),
 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)
6.d Fitted hexagon refined as free rotating group:
 C00N(C01G,C01R,C01T,C01U,C01S)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 452 electrons were 
found in a volume of 1700\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.875[CH2Cl2], 0.5[CH2Cl2] per ASU (7 + 4 CH2Cl2 per unit cell)
which account for 462 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_exptl_crystal_mounting_method 'glass fibre, Fromblin oil'
_olex2_submission_special_instructions 'No special instructions were received'