#------------------------------------------------------------------------------
#$Date: 2017-07-12 05:25:26 +0300 (Wed, 12 Jul 2017) $
#$Revision: 198659 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/35/7043579.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_7043579
loop_
_publ_author_name
'Lee, Kyounghoon'
'Donahue, Courtney M.'
'Daly, Scott R.'
_publ_section_title
;
 Triaminoborane-bridged diphosphine complexes with Ni and Pd: coordination
 chemistry, structures, and ligand-centered reactivity
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02144E
_journal_year                    2017
_chemical_formula_moiety         'C30 H32 B N3 P2, 2(C H2 Cl2)'
_chemical_formula_sum            'C32 H36 B Cl4 N3 P2'
_chemical_formula_weight         677.19
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-06-30 deposited with the CCDC.
2017-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.323(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.219(2)
_cell_length_b                   13.6886(14)
_cell_length_c                   13.9571(14)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.92
_cell_volume                     3375.8(6)
_computing_cell_refinement       'APEX II (Bruker-AXS, 2015)'
_computing_data_collection       'APEX II (Bruker-AXS, 2015)'
_computing_data_reduction        'APEX II (Bruker-AXS, 2015)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      190.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Nonius Kappa Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39293
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.032
_diffrn_reflns_theta_min         3.079
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.9677
_exptl_absorpt_correction_T_min  0.8991
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0331
_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)+(0.0362P)²+3.1561P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3379
_reflns_number_total             4062
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02144e2.cif
_cod_data_source_block           dal1538
_cod_database_code               7043579
_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   0.968
_shelx_estimated_absorpt_t_min   0.899
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26)
;
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_refinement_flags_occupancy
P1 P 0.09227(2) 0.56765(2) 0.34126(3) 0.02102(9) Uani 1 1 d . . .
N1 N 0.06196(6) 0.45961(8) 0.26449(10) 0.0228(2) Uani 1 1 d . . .
N2 N 0.000000 0.30452(12) 0.250000 0.0257(3) Uani 1 2 d S T P
B1 B 0.000000 0.40812(16) 0.250000 0.0217(4) Uani 1 2 d S T P
C1 C 0.11233(8) 0.39927(11) 0.25233(13) 0.0284(3) Uani 1 1 d . . .
H1A H 0.158577 0.436693 0.280943 0.034 Uiso 1 1 calc R . .
H1B H 0.086163 0.382586 0.166529 0.034 Uiso 1 1 calc R . .
C2 C 0.13379(9) 0.30638(11) 0.32569(14) 0.0332(3) Uani 1 1 d . . .
H2A H 0.159023 0.323184 0.411199 0.040 Uiso 1 1 calc R . .
H2B H 0.169813 0.268144 0.321147 0.040 Uiso 1 1 calc R . .
C3 C 0.06366(9) 0.24533(11) 0.27811(15) 0.0325(3) Uani 1 1 d . . .
H3A H 0.048738 0.210509 0.204472 0.039 Uiso 1 1 calc R . .
H3B H 0.075885 0.195668 0.339094 0.039 Uiso 1 1 calc R . .
C11 C 0.18655(7) 0.53411(10) 0.47848(12) 0.0221(3) Uani 1 1 d . . .
C12 C 0.25469(8) 0.53063(11) 0.49350(13) 0.0273(3) Uani 1 1 d . . .
H12 H 0.256662 0.554091 0.431394 0.033 Uiso 1 1 calc R . .
C13 C 0.31960(8) 0.49306(11) 0.59871(14) 0.0336(3) Uani 1 1 d . . .
H13 H 0.365640 0.491231 0.608027 0.040 Uiso 1 1 calc R . .
C14 C 0.31773(9) 0.45830(11) 0.68997(14) 0.0346(4) Uani 1 1 d . . .
H14 H 0.362199 0.432298 0.761406 0.042 Uiso 1 1 calc R . .
C15 C 0.25086(9) 0.46159(11) 0.67672(14) 0.0337(3) Uani 1 1 d . . .
H15 H 0.249117 0.437226 0.738729 0.040 Uiso 1 1 calc R . .
C16 C 0.18633(8) 0.50054(11) 0.57273(13) 0.0273(3) Uani 1 1 d . . .
H16 H 0.141029 0.504454 0.565467 0.033 Uiso 1 1 calc R . .
C21 C 0.11452(7) 0.64078(10) 0.25701(12) 0.0224(3) Uani 1 1 d . . .
C22 C 0.16520(8) 0.71908(10) 0.31274(13) 0.0289(3) Uani 1 1 d . . .
H22 H 0.192705 0.728706 0.397010 0.035 Uiso 1 1 calc R . .
C23 C 0.17595(9) 0.78285(11) 0.24714(15) 0.0355(4) Uani 1 1 d . . .
H23 H 0.210991 0.835175 0.286582 0.043 Uiso 1 1 calc R . .
C24 C 0.13561(10) 0.77014(12) 0.12422(15) 0.0384(4) Uani 1 1 d . . .
H24 H 0.143039 0.813614 0.079180 0.046 Uiso 1 1 calc R . .
C25 C 0.08445(9) 0.69417(12) 0.06691(14) 0.0357(4) Uani 1 1 d . . .
H25 H 0.056402 0.685896 -0.017660 0.043 Uiso 1 1 calc R . .
C26 C 0.07390(8) 0.62978(11) 0.13269(13) 0.0279(3) Uani 1 1 d . . .
H26 H 0.038653 0.577735 0.092556 0.033 Uiso 1 1 calc R . .
C31 C 0.05492(11) 0.17853(14) 0.91068(17) 0.0471(4) Uani 1 1 d . . .
H31A H 0.014445 0.228498 0.873708 0.057 Uiso 1 1 calc R . .
H31B H 0.071905 0.172214 0.859770 0.057 Uiso 1 1 calc R . .
Cl1 Cl 0.13105(3) 0.21729(4) 1.05495(4) 0.05474(14) Uani 1 1 d . . .
Cl2 Cl 0.01836(4) 0.06683(5) 0.91402(7) 0.0811(2) 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'
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'
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
_geom_angle_site_symmetry_3
N1 P1 C11 101.75(6) . .
N1 P1 C21 103.21(6) . .
C21 P1 C11 102.98(6) . .
B1 N1 P1 119.30(10) . .
B1 N1 C1 115.67(12) . .
C1 N1 P1 121.14(9) . .
B1 N2 C3 123.65(8) . .
B1 N2 C3 123.65(8) . 2
C3 N2 C3 112.70(16) 2 .
N1 B1 N1 121.72(18) 2 .
N2 B1 N1 119.14(9) . .
N2 B1 N1 119.14(9) . 2
N1 C1 H1A 109.7 . .
N1 C1 H1B 109.7 . .
N1 C1 C2 109.89(12) . .
H1A C1 H1B 108.2 . .
C2 C1 H1A 109.7 . .
C2 C1 H1B 109.7 . .
C1 C2 H2A 109.6 . .
C1 C2 H2B 109.6 . .
C1 C2 C3 110.27(12) . .
H2A C2 H2B 108.1 . .
C3 C2 H2A 109.6 . .
C3 C2 H2B 109.6 . .
N2 C3 C2 112.39(12) . .
N2 C3 H3A 109.1 . .
N2 C3 H3B 109.1 . .
C2 C3 H3A 109.1 . .
C2 C3 H3B 109.1 . .
H3A C3 H3B 107.9 . .
C12 C11 P1 127.54(11) . .
C16 C11 P1 114.18(10) . .
C16 C11 C12 118.02(13) . .
C11 C12 H12 119.8 . .
C13 C12 C11 120.45(14) . .
C13 C12 H12 119.8 . .
C12 C13 H13 119.7 . .
C14 C13 C12 120.56(14) . .
C14 C13 H13 119.7 . .
C13 C14 H14 120.1 . .
C15 C14 C13 119.70(14) . .
C15 C14 H14 120.1 . .
C14 C15 H15 120.1 . .
C14 C15 C16 119.87(14) . .
C16 C15 H15 120.1 . .
C11 C16 H16 119.3 . .
C15 C16 C11 121.37(14) . .
C15 C16 H16 119.3 . .
C22 C21 P1 120.17(11) . .
C26 C21 P1 121.18(11) . .
C26 C21 C22 117.99(13) . .
C21 C22 H22 119.4 . .
C23 C22 C21 121.17(14) . .
C23 C22 H22 119.4 . .
C22 C23 H23 120.1 . .
C24 C23 C22 119.90(15) . .
C24 C23 H23 120.1 . .
C23 C24 H24 120.0 . .
C25 C24 C23 119.97(15) . .
C25 C24 H24 120.0 . .
C24 C25 H25 119.9 . .
C24 C25 C26 120.21(14) . .
C26 C25 H25 119.9 . .
C21 C26 H26 119.6 . .
C25 C26 C21 120.74(14) . .
C25 C26 H26 119.6 . .
H31A C31 H31B 107.9 . .
Cl1 C31 H31A 109.2 . .
Cl1 C31 H31B 109.2 . .
Cl2 C31 H31A 109.2 . .
Cl2 C31 H31B 109.2 . .
Cl2 C31 Cl1 112.06(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 N1 1.7069(12) .
P1 C11 1.8446(14) .
P1 C21 1.8260(14) .
N1 B1 1.4475(15) .
N1 C1 1.4811(17) .
N2 B1 1.418(3) .
N2 C3 1.4624(17) .
N2 C3 1.4624(17) 2
B1 N1 1.4475(15) 2
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C1 C2 1.517(2) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C2 C3 1.521(2) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C11 C12 1.3977(19) .
C11 C16 1.3962(19) .
C12 H12 0.9500 .
C12 C13 1.390(2) .
C13 H13 0.9500 .
C13 C14 1.384(2) .
C14 H14 0.9500 .
C14 C15 1.382(2) .
C15 H15 0.9500 .
C15 C16 1.387(2) .
C16 H16 0.9500 .
C21 C22 1.3999(19) .
C21 C26 1.3960(19) .
C22 H22 0.9500 .
C22 C23 1.387(2) .
C23 H23 0.9500 .
C23 C24 1.383(2) .
C24 H24 0.9500 .
C24 C25 1.382(2) .
C25 H25 0.9500 .
C25 C26 1.391(2) .
C26 H26 0.9500 .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
C31 Cl1 1.7514(19) .
C31 Cl2 1.745(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_4
P1 N1 B1 N1 34.45(6) . 2
P1 N1 B1 N2 -145.55(6) . .
P1 N1 C1 C2 110.64(12) . .
P1 C11 C12 C13 -172.57(12) . .
P1 C11 C16 C15 172.29(12) . .
P1 C21 C22 C23 -172.03(12) . .
P1 C21 C26 C25 171.55(12) . .
N1 P1 C11 C12 84.07(13) . .
N1 P1 C11 C16 -89.84(11) . .
N1 P1 C21 C22 -157.14(11) . .
N1 P1 C21 C26 32.34(12) . .
N1 C1 C2 C3 62.55(15) . .
B1 N1 C1 C2 -46.99(15) . .
B1 N2 C3 C2 8.77(15) . .
C1 N1 B1 N1 -167.49(12) . 2
C1 N1 B1 N2 12.51(12) . .
C1 C2 C3 N2 -42.97(17) . .
C3 N2 B1 N1 -172.46(9) . 2
C3 N2 B1 N1 -172.46(9) 2 .
C3 N2 B1 N1 7.54(9) . .
C3 N2 B1 N1 7.54(9) 2 2
C3 N2 C3 C2 -171.23(15) 2 .
C11 P1 N1 B1 111.25(10) . .
C11 P1 N1 C1 -45.58(12) . .
C11 P1 C21 C22 -51.55(12) . .
C11 P1 C21 C26 137.92(11) . .
C11 C12 C13 C14 0.2(2) . .
C12 C11 C16 C15 -2.2(2) . .
C12 C13 C14 C15 -0.4(2) . .
C13 C14 C15 C16 -0.6(2) . .
C14 C15 C16 C11 2.0(2) . .
C16 C11 C12 C13 1.1(2) . .
C21 P1 N1 B1 -142.22(9) . .
C21 P1 N1 C1 60.95(12) . .
C21 P1 C11 C12 -22.64(14) . .
C21 P1 C11 C16 163.45(10) . .
C21 C22 C23 C24 0.7(2) . .
C22 C21 C26 C25 0.8(2) . .
C22 C23 C24 C25 0.2(3) . .
C23 C24 C25 C26 -0.6(3) . .
C24 C25 C26 C21 0.1(2) . .
C26 C21 C22 C23 -1.2(2) . .
