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#$Date: 2023-10-13 02:05:45 +0300 (Fri, 13 Oct 2023) $
#$Revision: 286943 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/41/7714196.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_7714196
loop_
_publ_author_name
'Kaniewska-Laskowska, Kinga'
'Ordyszewska, Anna'
'Wojnowski, Tomasz'
'Halenka, Hanna'
'Czapla, Marcin'
'Chojnacki, Jarosław'
'Grubba, Rafał'
_publ_section_title
;
 Phosphinoborenium cations stabilized by N-heterocyclic carbenes:
 synthesis, structure, and reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03090C
_journal_year                    2023
_chemical_formula_moiety         'C14 H32 Au B Br Cl N P'
_chemical_formula_sum            'C14 H32 Au B Br Cl N P'
_chemical_formula_weight         568.51
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-10-09 deposited with the CCDC.	2023-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.402(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9513(11)
_cell_length_b                   9.9691(9)
_cell_length_c                   17.3494(15)
_cell_measurement_reflns_used    17405
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.38
_cell_volume                     2065.3(3)
_computing_cell_refinement       'X-Area Recipe 1.34.0.0 (STOE, 2019)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction
'X-Area Integrate 1.77.0.0 (STOE, 2019) X-Area X-Red32 1.65.0.0 (STOE, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13321
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         2.350
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_exptl_absorpt_coefficient_mu    9.257
_exptl_absorpt_correction_T_max  0.4082
_exptl_absorpt_correction_T_min  0.1341
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.431
_refine_diff_density_min         -2.793
_refine_diff_density_rms         0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0574
_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)+(0.0883P)²+23.1650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4041
_reflns_number_total             4274
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03090c2.cif
_cod_data_source_block           1c
_cod_database_code               7714196
_shelx_shelxl_version_number     2018/3
_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   0.429
_shelx_estimated_absorpt_t_min   0.197
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C)
;
_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
Au1 Au 0.24464(2) 0.60220(3) 0.47039(2) 0.02179(15) Uani 1 1 d . . . . .
Br1 Br 0.23736(8) 0.73480(10) 0.58610(5) 0.0350(2) Uani 1 1 d . . . . .
Cl1 Cl 0.31067(18) 0.1929(2) 0.29129(12) 0.0284(4) Uani 1 1 d . . . . .
P1 P 0.25349(15) 0.4815(2) 0.35997(11) 0.0178(4) Uani 1 1 d . . . . .
N1 N 0.2313(5) 0.2151(7) 0.4387(4) 0.0198(13) Uani 1 1 d . . . . .
C1 C 0.3876(7) 0.5356(9) 0.3134(5) 0.0271(17) Uani 1 1 d . . . . .
C2 C 0.4823(7) 0.4650(11) 0.3601(6) 0.034(2) Uani 1 1 d . . . . .
H2A H 0.471010 0.476566 0.415358 0.051 Uiso 1 1 calc GR . . . .
H2B H 0.554398 0.504146 0.347313 0.051 Uiso 1 1 calc GR . . . .
H2C H 0.481971 0.369137 0.347549 0.051 Uiso 1 1 calc GR . . . .
C3 C 0.3952(8) 0.5032(9) 0.2282(5) 0.0303(18) Uani 1 1 d . . . . .
H3A H 0.383956 0.406703 0.220125 0.045 Uiso 1 1 calc GR . . . .
H3B H 0.469195 0.528892 0.210872 0.045 Uiso 1 1 calc GR . . . .
H3C H 0.337275 0.552985 0.198503 0.045 Uiso 1 1 calc GR . . . .
C4 C 0.4025(9) 0.6881(10) 0.3243(6) 0.039(2) Uani 1 1 d . . . . .
H4A H 0.339053 0.735116 0.298947 0.058 Uiso 1 1 calc GR . . . .
H4B H 0.472179 0.716735 0.301420 0.058 Uiso 1 1 calc GR . . . .
H4C H 0.405752 0.709428 0.379506 0.058 Uiso 1 1 calc GR . . . .
C5 C 0.1226(7) 0.5085(8) 0.2981(5) 0.0219(15) Uani 1 1 d . . . . .
C6 C 0.1202(8) 0.4351(10) 0.2213(5) 0.0324(19) Uani 1 1 d . . . . .
H6A H 0.176638 0.473691 0.188394 0.049 Uiso 1 1 calc GR . . . .
H6B H 0.045855 0.444506 0.195799 0.049 Uiso 1 1 calc GR . . . .
H6C H 0.136511 0.339903 0.230082 0.049 Uiso 1 1 calc GR . . . .
C7 C 0.1059(8) 0.6588(9) 0.2826(5) 0.0314(18) Uani 1 1 d . . . . .
H7A H 0.109828 0.707775 0.331643 0.047 Uiso 1 1 calc GR . . . .
H7B H 0.032393 0.673431 0.256752 0.047 Uiso 1 1 calc GR . . . .
H7C H 0.164623 0.691285 0.249580 0.047 Uiso 1 1 calc GR . . . .
C8 C 0.0266(6) 0.4586(9) 0.3465(5) 0.0278(17) Uani 1 1 d . . . . .
H8A H 0.037526 0.363199 0.358273 0.042 Uiso 1 1 calc GR . . . .
H8B H -0.044773 0.470732 0.317398 0.042 Uiso 1 1 calc GR . . . .
H8C H 0.025629 0.509772 0.394646 0.042 Uiso 1 1 calc GR . . . .
C9 C 0.1816(8) 0.2795(9) 0.5053(5) 0.0299(18) Uani 1 1 d . . . . .
H9 H 0.165219 0.374391 0.489884 0.036 Uiso 1 1 calc R . . . .
C10 C 0.2599(10) 0.2858(11) 0.5747(5) 0.043(3) Uani 1 1 d . . . . .
H10A H 0.276032 0.194735 0.593224 0.064 Uiso 1 1 calc GR . . . .
H10B H 0.225202 0.337463 0.615390 0.064 Uiso 1 1 calc GR . . . .
H10C H 0.329783 0.329459 0.560908 0.064 Uiso 1 1 calc GR . . . .
C11 C 0.0694(8) 0.2159(10) 0.5241(6) 0.035(2) Uani 1 1 d . . . . .
H11A H 0.019834 0.215072 0.477644 0.052 Uiso 1 1 calc GR . . . .
H11B H 0.034673 0.268255 0.564503 0.052 Uiso 1 1 calc GR . . . .
H11C H 0.081884 0.123793 0.542154 0.052 Uiso 1 1 calc GR . . . .
C12 C 0.2493(7) 0.0654(10) 0.4516(6) 0.0299(18) Uani 1 1 d . . . . .
H12 H 0.226418 0.046303 0.505277 0.036 Uiso 1 1 calc R . . . .
C13 C 0.1746(8) -0.0191(10) 0.3988(6) 0.037(2) Uani 1 1 d . . . . .
H13A H 0.096359 0.007281 0.404388 0.055 Uiso 1 1 calc GR . . . .
H13B H 0.183811 -0.113964 0.412576 0.055 Uiso 1 1 calc GR . . . .
H13C H 0.195061 -0.005616 0.345280 0.055 Uiso 1 1 calc GR . . . .
C14 C 0.3737(8) 0.0254(11) 0.4490(8) 0.045(3) Uani 1 1 d . . . . .
H14A H 0.395588 0.022108 0.395213 0.067 Uiso 1 1 calc GR . . . .
H14B H 0.384696 -0.063072 0.472724 0.067 Uiso 1 1 calc GR . . . .
H14C H 0.419773 0.091735 0.477341 0.067 Uiso 1 1 calc GR . . . .
B1 B 0.2604(8) 0.2845(9) 0.3743(5) 0.0220(17) 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'
Au Au -2.0133 8.8022 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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
P1 Au1 Br1 178.63(6) . . ?
C1 P1 Au1 106.1(3) . . ?
C1 P1 B1 107.7(4) . . ?
C5 P1 Au1 109.8(3) . . ?
C5 P1 C1 114.4(4) . . ?
C5 P1 B1 104.1(4) . . ?
B1 P1 Au1 115.0(3) . . ?
C9 N1 C12 111.9(7) . . ?
B1 N1 C9 123.0(7) . . ?
B1 N1 C12 125.1(7) . . ?
C2 C1 P1 105.2(6) . . ?
C2 C1 C4 108.0(7) . . ?
C3 C1 P1 116.0(6) . . ?
C3 C1 C2 110.1(7) . . ?
C3 C1 C4 108.5(7) . . ?
C4 C1 P1 108.8(6) . . ?
C6 C5 P1 114.6(6) . . ?
C6 C5 C7 108.6(7) . . ?
C6 C5 C8 109.7(7) . . ?
C7 C5 P1 109.9(6) . . ?
C8 C5 P1 105.4(5) . . ?
C8 C5 C7 108.5(7) . . ?
N1 C9 C10 113.1(8) . . ?
N1 C9 C11 111.9(7) . . ?
C10 C9 C11 111.7(8) . . ?
N1 C12 C14 112.3(7) . . ?
C13 C12 N1 112.4(7) . . ?
C13 C12 C14 112.6(9) . . ?
Cl1 B1 P1 114.2(5) . . ?
N1 B1 Cl1 119.5(6) . . ?
N1 B1 P1 126.3(7) . . ?
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
Au1 Br1 2.4082(9) . ?
Au1 P1 2.2688(19) . ?
Cl1 B1 1.829(10) . ?
P1 C1 1.903(9) . ?
P1 C5 1.879(8) . ?
P1 B1 1.980(9) . ?
N1 C9 1.468(10) . ?
N1 C12 1.524(12) . ?
N1 B1 1.371(11) . ?
C1 C2 1.535(12) . ?
C1 C3 1.521(13) . ?
C1 C4 1.542(13) . ?
C5 C6 1.520(12) . ?
C5 C7 1.534(12) . ?
C5 C8 1.533(11) . ?
C9 C10 1.495(13) . ?
C9 C11 1.531(12) . ?
C12 C13 1.509(13) . ?
C12 C14 1.541(12) . ?
