#------------------------------------------------------------------------------
#$Date: 2019-11-26 07:15:43 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242926 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/30/4133079.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_4133079
loop_
_publ_author_name
'Muessig, Jonas H.'
'Prieschl, Dominic'
'Deißenberger, Andrea'
'Dewhurst, Rian D.'
'Dietz, Maximilian'
'Jiménez-Halla, J Oscar C'
'Trumpp, Alexandra'
'Wang, Sunewang R.'
'Brunecker, Carina'
'Haefner, Alena'
'Gärtner, Annalena'
'Thiess, Torsten'
'Böhnke, Julian'
'Radacki, Krzysztof'
'Bertermann, Rüdiger'
'Marder, Todd B.'
'Braunschweig, Holger'
_publ_section_title
;
 Reactivity of Tetrahalo- and Difluorodiboranes(4) toward Lewis Basic
 Platinum(0): Bis(boryl), Borylborato, and Doubly Boryl-Bridged Platinum
 Complexes.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13056
_journal_page_last               13063
_journal_paper_doi               10.1021/jacs.8b08428
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C6 H18 B2 Cl4 P2'
_chemical_formula_sum            'C6 H18 B2 Cl4 P2'
_chemical_formula_weight         315.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_secondary   iterative
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 95.955(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4637(16)
_cell_length_b                   12.672(4)
_cell_length_c                   8.946(3)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      2.80
_cell_volume                     728.8(4)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CMOS area detector (Photon 100)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0115
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            23447
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         2.797
_diffrn_source                   'microfocus sealed tube (Incoatec ImS)'
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0174
_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)+(0.0205P)²+0.2905P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1378
_reflns_number_total             1490
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b08428_si_012.cif
_cod_data_source_block           B2Cl4(PMe3)2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4133079
_shelx_shelxl_version_number     2014/7
_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_min   0.857
_shelx_estimated_absorpt_t_max   0.951
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Cl1 Cl 0.65198(4) 0.40577(2) 0.31047(3) 0.01374(8) Uani 1 1 d . .
C1 C 0.54186(19) 0.63778(10) 0.12126(13) 0.0173(3) Uani 1 1 d . .
H1A H 0.6041 0.5739 0.0833 0.026 Uiso 1 1 calc R U
H1B H 0.6522 0.6870 0.1586 0.026 Uiso 1 1 calc R U
H1C H 0.4518 0.6712 0.0399 0.026 Uiso 1 1 calc R U
P1 P 0.39004(4) 0.60323(2) 0.27210(3) 0.01104(9) Uani 1 1 d . .
B1 B 0.56055(18) 0.52034(10) 0.42392(14) 0.0107(2) Uani 1 1 d . .
Cl2 Cl 0.78711(4) 0.61147(2) 0.47867(3) 0.01528(8) Uani 1 1 d . .
C2 C 0.16395(18) 0.53476(10) 0.18617(14) 0.0189(3) Uani 1 1 d . .
H2A H 0.0976 0.5770 0.1028 0.028 Uiso 1 1 calc R U
H2B H 0.0654 0.5237 0.2609 0.028 Uiso 1 1 calc R U
H2C H 0.2058 0.4663 0.1481 0.028 Uiso 1 1 calc R U
C3 C 0.2987(2) 0.72553(10) 0.34249(14) 0.0214(3) Uani 1 1 d . .
H3A H 0.2306 0.7670 0.2589 0.032 Uiso 1 1 calc R U
H3B H 0.4167 0.7654 0.3916 0.032 Uiso 1 1 calc R U
H3C H 0.1991 0.7110 0.4153 0.032 Uiso 1 1 calc R U
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'
Cl Cl 0.1484 0.1585 '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
P1 C1 H1A 109.5 .
P1 C1 H1B 109.5 .
H1A C1 H1B 109.5 .
P1 C1 H1C 109.5 .
H1A C1 H1C 109.5 .
H1B C1 H1C 109.5 .
C3 P1 C2 106.48(6) .
C3 P1 C1 106.09(6) .
C2 P1 C1 106.14(6) .
C3 P1 B1 113.62(6) .
C2 P1 B1 114.20(6) .
C1 P1 B1 109.74(6) .
B1 B1 Cl2 112.49(10) 3_666
B1 B1 Cl1 112.72(11) 3_666
Cl2 B1 Cl1 109.26(6) .
B1 B1 P1 116.07(10) 3_666
Cl2 B1 P1 102.52(6) .
Cl1 B1 P1 102.87(6) .
P1 C2 H2A 109.5 .
P1 C2 H2B 109.5 .
H2A C2 H2B 109.5 .
P1 C2 H2C 109.5 .
H2A C2 H2C 109.5 .
H2B C2 H2C 109.5 .
P1 C3 H3A 109.5 .
P1 C3 H3B 109.5 .
H3A C3 H3B 109.5 .
P1 C3 H3C 109.5 .
H3A C3 H3C 109.5 .
H3B C3 H3C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 B1 1.9004(13) .
C1 P1 1.8029(13) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
P1 C3 1.7955(13) .
P1 C2 1.8017(12) .
P1 B1 1.9626(13) .
B1 B1 1.718(3) 3_666
B1 Cl2 1.8892(13) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
