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_7714172
_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         '2(C13 H26 B Cl P Rh), C16 H24 Cl2 Rh2'
_chemical_formula_sum            'C42 H76 B2 Cl4 P2 Rh4'
_chemical_formula_weight         1218.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-12
_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                63.032(2)
_cell_angle_beta                 87.633(2)
_cell_angle_gamma                77.146(2)
_cell_formula_units_Z            1
_cell_length_a                   9.1435(5)
_cell_length_b                   11.7779(6)
_cell_length_c                   12.7866(6)
_cell_measurement_reflns_used    6965
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      34.20
_cell_measurement_theta_min      2.67
_cell_volume                     1193.70(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9297
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.561
_diffrn_reflns_theta_min         1.791
_exptl_absorpt_coefficient_mu    1.678
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.6786
_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 0.0455 before and 0.0355 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0863 before and 0.0556 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 87040 reflections, Rint = 0.0383
 (37221 with I > 3sig(I), Rint = 0.0303)
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         9297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0303P)^2^+0.9303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8521
_reflns_number_total             9297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02538a3.cif
_cod_data_source_block           RhClCODMePB_RhClCOD
_cod_database_code               7714172
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.651
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8795(3)
 0.1205(3)
2. 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
3.a Ternary CH refined with riding coordinates:
 C10(H10), C11(H11), C6(H6), C7(H7), C19(H19), C18(H18), C15(H15), C14(H14)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C1(H1A,H1B), C12(H12A,H12B), C13(H13A,H13B), C8(H8A,H8B),
 C17(H17A,H17B), C16(H16A,H16B), C21(H21A,H21B), C20(H20A,H20B)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              54954
_olex2_submission_special_instructions 'No special instructions were received'