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#$Date: 2023-10-11 01:55:58 +0300 (Wed, 11 Oct 2023) $
#$Revision: 286882 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/41/7714169.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7714169
loop_
_publ_author_name
'Paskaruk, Katia M.'
'Emslie, David J. H.'
'Britten, James F.'
_publ_section_title
;
 A comparison of the coordination behaviour of
 R₂PCH₂BMe₂ (R = Me vs. 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         'C30 H36 B2 P2'
_chemical_formula_sum            'C30 H36 B2 P2'
_chemical_formula_weight         480.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_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                 110.905(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8122(7)
_cell_length_b                   13.4175(10)
_cell_length_c                   9.8646(7)
_cell_measurement_reflns_used    2661
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      23.954
_cell_measurement_theta_min      2.524
_cell_volume                     1336.88(17)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33141
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.569
_diffrn_reflns_theta_min         2.016
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6884
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0577 before and 0.0532 after correction.
The Ratio of minimum to maximum transmission is 0.9227.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0460
_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/[σ²(Fo²)+(0.0499P)²+0.3238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2930
_reflns_number_total             4081
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02538a3.cif
_cod_data_source_block           PhPBMe
_cod_database_code               7714169
_shelx_shelxl_version_number     2019/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.965
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.36228(4) 0.51984(3) 0.84055(4) 0.01641(11) Uani 1 1 d . . . . .
C1 C 0.23755(14) 0.59619(11) 0.87696(16) 0.0186(3) Uani 1 1 d . . . . .
C2 C 0.20550(16) 0.69091(13) 0.81453(18) 0.0245(3) Uani 1 1 d . . . . .
H2 H 0.2472(18) 0.7169(14) 0.755(2) 0.029(5) Uiso 1 1 d . . . . .
C3 C 0.11140(17) 0.74928(13) 0.8444(2) 0.0280(4) Uani 1 1 d . . . . .
H3 H 0.089(2) 0.8104(17) 0.805(2) 0.040(6) Uiso 1 1 d . . . . .
C4 C 0.04838(16) 0.71420(13) 0.93475(19) 0.0265(4) Uani 1 1 d . . . . .
H4 H -0.012(2) 0.7538(16) 0.955(2) 0.036(5) Uiso 1 1 d . . . . .
C5 C 0.07934(16) 0.62044(13) 0.99678(18) 0.0258(3) Uani 1 1 d . . . . .
H5 H 0.0369(19) 0.5941(16) 1.059(2) 0.038(5) Uiso 1 1 d . . . . .
C6 C 0.17386(15) 0.56166(13) 0.96849(17) 0.0229(3) Uani 1 1 d . . . . .
H6 H 0.1959(18) 0.4983(14) 1.011(2) 0.021(5) Uiso 1 1 d . . . . .
C7 C 0.29553(15) 0.50738(11) 0.64315(16) 0.0189(3) Uani 1 1 d . . . . .
C8 C 0.17530(16) 0.45636(13) 0.57842(18) 0.0250(3) Uani 1 1 d . . . . .
H8 H 0.1275(18) 0.4347(15) 0.639(2) 0.029(5) Uiso 1 1 d . . . . .
C9 C 0.12574(17) 0.43871(13) 0.42981(18) 0.0272(4) Uani 1 1 d . . . . .
H9 H 0.045(2) 0.4085(17) 0.387(2) 0.047(6) Uiso 1 1 d . . . . .
C10 C 0.19379(17) 0.47255(13) 0.34353(18) 0.0282(4) Uani 1 1 d . . . . .
H10 H 0.159(2) 0.4581(15) 0.239(2) 0.038(6) Uiso 1 1 d . . . . .
C11 C 0.31060(18) 0.52567(15) 0.40523(18) 0.0297(4) Uani 1 1 d . . . . .
H11 H 0.358(2) 0.5501(16) 0.345(2) 0.040(6) Uiso 1 1 d . . . . .
C12 C 0.36158(16) 0.54287(13) 0.55485(18) 0.0247(3) Uani 1 1 d . . . . .
H12 H 0.4399(19) 0.5780(14) 0.596(2) 0.030(5) Uiso 1 1 d . . . . .
C13 C 0.51065(14) 0.59513(12) 0.88960(16) 0.0187(3) Uani 1 1 d . . . . .
H13A H 0.5680(18) 0.5620(14) 0.844(2) 0.029(5) Uiso 1 1 d . . . . .
H13B H 0.4849(19) 0.6594(15) 0.840(2) 0.033(5) Uiso 1 1 d . . . . .
C14 C 0.50554(17) 0.66577(13) 1.15110(18) 0.0246(3) Uani 1 1 d . . . . .
H14A H 0.5601(18) 0.6832(14) 1.253(2) 0.029(5) Uiso 1 1 d . . . . .
H14B H 0.466(2) 0.7314(16) 1.098(2) 0.039(6) Uiso 1 1 d . . . . .
H14C H 0.432(2) 0.6249(15) 1.156(2) 0.035(5) Uiso 1 1 d . . . . .
C15 C 0.72272(17) 0.68383(13) 1.0837(2) 0.0285(4) Uani 1 1 d . . . . .
H15A H 0.690(2) 0.7543(17) 1.042(2) 0.046(6) Uiso 1 1 d . . . . .
H15B H 0.776(2) 0.6584(17) 1.027(3) 0.049(6) Uiso 1 1 d . . . . .
H15C H 0.785(2) 0.6953(16) 1.191(2) 0.044(6) Uiso 1 1 d . . . . .
B1 B 0.59340(16) 0.61502(13) 1.06483(19) 0.0193(3) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 B1 118.86(7) . 3_667 ?
C7 P1 C1 102.83(7) . . ?
C7 P1 B1 110.48(7) . 3_667 ?
C13 P1 C1 106.28(7) . . ?
C13 P1 C7 108.15(7) . . ?
C13 P1 B1 109.64(7) . 3_667 ?
C2 C1 P1 120.40(12) . . ?
C6 C1 P1 120.65(12) . . ?
C6 C1 C2 118.94(14) . . ?
C1 C2 H2 121.3(12) . . ?
C3 C2 C1 120.04(16) . . ?
C3 C2 H2 118.6(12) . . ?
C2 C3 H3 121.8(14) . . ?
C4 C3 C2 120.58(16) . . ?
C4 C3 H3 117.6(14) . . ?
C3 C4 H4 119.8(13) . . ?
C3 C4 C5 119.75(16) . . ?
C5 C4 H4 120.4(13) . . ?
C4 C5 H5 121.5(13) . . ?
C4 C5 C6 120.20(16) . . ?
C6 C5 H5 118.3(13) . . ?
C1 C6 H6 119.0(11) . . ?
C5 C6 C1 120.49(15) . . ?
C5 C6 H6 120.5(11) . . ?
C8 C7 P1 118.60(12) . . ?
C12 C7 P1 122.66(12) . . ?
C12 C7 C8 118.69(15) . . ?
C7 C8 H8 118.7(11) . . ?
C9 C8 C7 120.56(16) . . ?
C9 C8 H8 120.7(11) . . ?
C8 C9 H9 120.6(14) . . ?
C10 C9 C8 120.19(16) . . ?
C10 C9 H9 119.1(13) . . ?
C9 C10 H10 119.6(12) . . ?
C9 C10 C11 119.92(16) . . ?
C11 C10 H10 120.5(12) . . ?
C10 C11 H11 120.2(13) . . ?
C10 C11 C12 120.14(16) . . ?
C12 C11 H11 119.6(13) . . ?
C7 C12 C11 120.45(16) . . ?
C7 C12 H12 119.4(12) . . ?
C11 C12 H12 120.2(12) . . ?
P1 C13 H13A 105.5(11) . . ?
P1 C13 H13B 106.9(11) . . ?
H13A C13 H13B 106.2(16) . . ?
B1 C13 P1 117.72(10) . . ?
B1 C13 H13A 110.6(11) . . ?
B1 C13 H13B 109.3(12) . . ?
H14A C14 H14B 107.5(16) . . ?
H14A C14 H14C 106.0(16) . . ?
H14B C14 H14C 107.8(16) . . ?
B1 C14 H14A 112.3(11) . . ?
B1 C14 H14B 107.5(11) . . ?
B1 C14 H14C 115.4(12) . . ?
H15A C15 H15B 105.9(17) . . ?
H15A C15 H15C 105.9(17) . . ?
H15B C15 H15C 109.0(18) . . ?
B1 C15 H15A 108.2(12) . . ?
B1 C15 H15B 112.8(13) . . ?
B1 C15 H15C 114.6(12) . . ?
C13 B1 P1 106.79(10) . 3_667 ?
C14 B1 P1 102.68(11) . 3_667 ?
C14 B1 C13 114.33(13) . . ?
C15 B1 P1 113.80(11) . 3_667 ?
C15 B1 C13 109.37(13) . . ?
C15 B1 C14 109.82(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C1 1.8284(15) . ?
P1 C7 1.8269(15) . ?
P1 C13 1.8094(15) . ?
P1 B1 2.0139(18) 3_667 ?
C1 C2 1.401(2) . ?
C1 C6 1.396(2) . ?
C2 H2 0.927(19) . ?
C2 C3 1.396(2) . ?
C3 H3 0.90(2) . ?
C3 C4 1.383(3) . ?
C4 H4 0.92(2) . ?
C4 C5 1.387(2) . ?
C5 H5 0.96(2) . ?
C5 C6 1.396(2) . ?
C6 H6 0.942(18) . ?
C7 C8 1.405(2) . ?
C7 C12 1.393(2) . ?
C8 H8 0.962(19) . ?
C8 C9 1.390(2) . ?
C9 H9 0.92(2) . ?
C9 C10 1.385(3) . ?
C10 H10 0.99(2) . ?
C10 C11 1.387(3) . ?
C11 H11 0.97(2) . ?
C11 C12 1.398(2) . ?
C12 H12 0.93(2) . ?
C13 H13A 0.990(19) . ?
C13 H13B 0.98(2) . ?
C13 B1 1.660(2) . ?
C14 H14A 0.996(19) . ?
C14 H14B 1.04(2) . ?
C14 H14C 0.99(2) . ?
C14 B1 1.633(2) . ?
C15 H15A 1.04(2) . ?
C15 H15B 0.99(2) . ?
C15 H15C 1.04(2) . ?
C15 B1 1.630(2) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 C3 -179.15(12) . . . . ?
P1 C1 C6 C5 179.57(12) . . . . ?
P1 C7 C8 C9 -175.25(13) . . . . ?
P1 C7 C12 C11 175.73(13) . . . . ?
P1 C13 B1 P1 56.28(13) . . . 3_667 ?
P1 C13 B1 C14 -56.55(17) . . . . ?
P1 C13 B1 C15 179.84(11) . . . . ?
C1 P1 C7 C8 -64.26(14) . . . . ?
C1 P1 C7 C12 118.38(14) . . . . ?
C1 P1 C13 B1 71.92(12) . . . . ?
C1 C2 C3 C4 -0.4(3) . . . . ?
C2 C1 C6 C5 0.3(2) . . . . ?
C2 C3 C4 C5 0.3(3) . . . . ?
C3 C4 C5 C6 0.1(3) . . . . ?
C4 C5 C6 C1 -0.4(2) . . . . ?
C6 C1 C2 C3 0.1(2) . . . . ?
C7 P1 C1 C2 -58.48(14) . . . . ?
C7 P1 C1 C6 122.24(13) . . . . ?
C7 P1 C13 B1 -178.25(11) . . . . ?
C7 C8 C9 C10 -0.9(3) . . . . ?
C8 C7 C12 C11 -1.6(2) . . . . ?
C8 C9 C10 C11 -1.1(3) . . . . ?
C9 C10 C11 C12 1.7(3) . . . . ?
C10 C11 C12 C7 -0.3(3) . . . . ?
C12 C7 C8 C9 2.2(2) . . . . ?
C13 P1 C1 C2 55.05(14) . . . . ?
C13 P1 C1 C6 -124.22(13) . . . . ?
C13 P1 C7 C8 -176.43(12) . . . . ?
C13 P1 C7 C12 6.22(15) . . . . ?
B1 P1 C1 C2 179.15(12) 3_667 . . . ?
B1 P1 C1 C6 -0.12(16) 3_667 . . . ?
B1 P1 C7 C8 63.58(14) 3_667 . . . ?
B1 P1 C7 C12 -113.78(14) 3_667 . . . ?
B1 P1 C13 B1 -57.72(15) 3_667 . . . ?
