A comparison of the coordination behaviour of R<sub>2</sub>PCH<sub>2</sub>BMe<sub>2</sub> (R = Me <i>vs.</i> Ph) ambiphilic ligands with late transition metals.
Paskaruk, Katia M.; Emslie, David J. H.; Britten, James F.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt02538a

data_7714171
_publ_section_title
;
 A comparison of the coordination behaviour of
 R<sub>2</sub>PCH<sub>2</sub>BMe<sub>2</sub> (R = Me <i>vs.</i> Ph)
 ambiphilic ligands with late transition metals.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt02538a
_journal_year                    2023
_chemical_formula_moiety         'C10 H28 B2 Cl2 P2 Pt'
_chemical_formula_sum            'C10 H28 B2 Cl2 P2 Pt'
_chemical_formula_weight         497.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-18 deposited with the CCDC.	2023-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.64(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.677(2)
_cell_length_b                   21.878(4)
_cell_length_c                   15.393(3)
_cell_measurement_reflns_used    2225
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      22.671
_cell_measurement_theta_min      2.847
_cell_volume                     3655.3(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0858
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21881
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.588
_diffrn_reflns_theta_min         1.862
_diffrn_source_current           90.0
_diffrn_source_power             4.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.124
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0909 before and 0.0363 after correction.
 
For component 2:
 wR2(int) was 0.0976 before and 0.0464 after correction.
 The Ratio of minimum to maximum transmission is 0.62.

Final HKLF 4 output contains 41553 reflections, Rint = 0.0836
 (10417 with I > 3sig(I), Rint = 0.0602)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.809
_exptl_crystal_description       plate
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.159
_refine_diff_density_min         -1.842
_refine_diff_density_rms         0.266
_refine_ls_abs_structure_details
;
 Flack x determined using 3693 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         9657
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0666P)^2^+20.3505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1361
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_full    0.921
_reflns_Friedel_fraction_max     0.881
_reflns_number_gt                8912
_reflns_number_total             9657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02538a3.cif
_cod_data_source_block           PtCl2(MePB)2
_cod_database_code               7714171
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.293
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9069(18)
 0.0931(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B), C1A(H1AA,H1AB), C6A(H6AA,H6AB)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C2A(H2AA,H2AB,
 H2AC), C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C7A(H7AA,
 H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              48970
_olex2_submission_special_instructions 'No special instructions were received'