#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:54:20 +0100 (vie 25 de mar de 2016) $
#$Revision: 179735 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/31/7003133.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_7003133
loop_
_publ_author_name
'Hinchliffe, Alan'
'Mair, Francis S.'
'McInnes, Eric J. L.'
'Pritchard, Robin G.'
'Warren, John E.'
_publ_section_title
;
 Light group 13 chloride diazadiene complexes: consequences of varying
 substituent bulk
;
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              222
_journal_page_last               233
_journal_paper_doi               10.1039/b712911d
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H35 B1 Cl2 N2'
_chemical_formula_sum            'C26 H35 B Cl2 N2'
_chemical_formula_weight         457.27
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-07-18T22:46:31-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7771(5)
_cell_length_b                   20.7881(9)
_cell_length_c                   10.9245(5)
_cell_measurement_reflns_used    126592
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     2674.6(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.573095E-1
_diffrn_orient_matrix_UB_12      0.577953E-1
_diffrn_orient_matrix_UB_13      0.183787E-1
_diffrn_orient_matrix_UB_21      0.713608E-1
_diffrn_orient_matrix_UB_22      -0.472578E-1
_diffrn_orient_matrix_UB_23      -0.137966E-1
_diffrn_orient_matrix_UB_31      0.15352E-2
_diffrn_orient_matrix_UB_32      0.404501E-1
_diffrn_orient_matrix_UB_33      -0.422601E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19705
_diffrn_reflns_reduction_process
;
Scaled and merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.9685
_exptl_absorpt_correction_T_min  0.8984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'pale purple'
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.038(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.053
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0485P)²+1.0761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                1986
_reflns_number_total             2762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b712911d.txt
_cod_data_source_block           4
_cod_database_code               7003133
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.27407(5) 0.75 0.66073(6) 0.05714(17) Uani 1 d S . .
Cl2 Cl -0.15084(7) 0.67883(4) 0.49549(9) 0.0596(2) Uani 0.5 d P . .
N1 N 0.06642(11) 0.69512(7) 0.57937(11) 0.0462(3) Uani 1 d . . .
B1 B 0.1336(2) 0.75 0.6064(2) 0.0427(6) Uani 1 d S . .
C2 C -0.03832(14) 0.71842(10) 0.53714(15) 0.0558(5) Uani 1 d . . .
C10 C 0.09654(13) 0.62828(8) 0.57376(15) 0.0496(4) Uani 1 d . . .
C11 C 0.15005(14) 0.60540(9) 0.46768(16) 0.0559(5) Uani 1 d . . .
C12 C 0.17634(16) 0.54013(10) 0.46351(18) 0.0662(5) Uani 1 d . . .
C13 C 0.15085(17) 0.49984(10) 0.5592(2) 0.0689(6) Uani 1 d . . .
C14 C 0.09869(17) 0.52365(10) 0.66181(19) 0.0652(5) Uani 1 d . . .
C15 C 0.06965(14) 0.58812(9) 0.67212(16) 0.0542(4) Uani 1 d . . .
C16 C 0.01123(17) 0.61327(10) 0.78541(17) 0.0628(5) Uani 1 d . . .
C17 C 0.0925(3) 0.6218(2) 0.8892(3) 0.1479(16) Uani 1 d . . .
C18 C -0.0962(2) 0.57747(15) 0.8140(3) 0.1092(9) Uani 1 d . . .
C19 C 0.17941(18) 0.64878(11) 0.36163(17) 0.0656(5) Uani 1 d . . .
C20 C 0.1230(3) 0.62540(18) 0.2431(2) 0.1092(10) Uani 1 d . . .
C21 C 0.3061(2) 0.65459(14) 0.3428(2) 0.0881(8) Uani 1 d . . .
H10 H -0.0119(17) 0.6545(10) 0.7729(17) 0.073(6) Uiso 1 d . . .
H12 H 0.2142(15) 0.5252(9) 0.3935(16) 0.061(5) Uiso 1 d . . .
H13 H 0.1693(17) 0.4521(11) 0.5480(18) 0.081(6) Uiso 1 d . . .
H14 H 0.0802(16) 0.4962(9) 0.7244(17) 0.067(6) Uiso 1 d . . .
H17A H 0.0788(14) 0.5742(7) 0.9042(14) 0.037(4) Uiso 1 d . . .
H17B H 0.049(3) 0.6391(16) 0.973(3) 0.169(13) Uiso 1 d . . .
H17C H 0.166(3) 0.6238(17) 0.887(3) 0.161(14) Uiso 1 d . . .
H18A H -0.054(2) 0.5399(13) 0.852(2) 0.121(10) Uiso 1 d . . .
H18B H -0.127(2) 0.5970(13) 0.890(3) 0.113(9) Uiso 1 d . . .
H18C H -0.153(4) 0.566(3) 0.766(5) 0.27(3) Uiso 1 d . . .
H19 H 0.1534(17) 0.6883(10) 0.3771(18) 0.073(6) Uiso 1 d . . .
H20A H 0.134(2) 0.6552(13) 0.181(2) 0.119(9) Uiso 1 d . . .
H20B H 0.040(3) 0.6284(14) 0.265(3) 0.140(11) Uiso 1 d . . .
H20C H 0.174(6) 0.572(3) 0.228(6) 0.33(3) Uiso 1 d . . .
H21A H 0.325(2) 0.6812(12) 0.269(2) 0.107(8) Uiso 1 d . . .
H21B H 0.346(2) 0.6658(14) 0.420(3) 0.121(9) Uiso 1 d . . .
H21C H 0.333(3) 0.6120(14) 0.316(3) 0.127(10) Uiso 1 d . . .
H2 H -0.079(4) 0.6859(19) 0.522(4) 0.062(11) Uiso 0.5 d P A 1
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 0 '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'
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
_geom_angle_publ_flag
C2 N1 B1 106.32(14) . . ?
C2 N1 C10 122.50(14) . . ?
B1 N1 C10 130.48(14) . . ?
N1 B1 N1 106.97(19) . 8_575 ?
N1 B1 Cl1 126.51(10) . . ?
N1 B1 Cl1 126.51(10) 8_575 . ?
C2 C2 N1 110.19(10) 8_575 . ?
C2 C2 Cl2 120.43(7) 8_575 . ?
N1 C2 Cl2 129.36(15) . . ?
C15 C10 C11 122.33(16) . . ?
C15 C10 N1 119.31(15) . . ?
C11 C10 N1 118.34(15) . . ?
C12 C11 C10 117.23(17) . . ?
C12 C11 C19 120.43(17) . . ?
C10 C11 C19 122.34(17) . . ?
C13 C12 C11 121.40(18) . . ?
C14 C13 C12 120.03(19) . . ?
C13 C14 C15 121.71(19) . . ?
C14 C15 C10 117.31(17) . . ?
C14 C15 C16 120.89(17) . . ?
C10 C15 C16 121.80(16) . . ?
C17 C16 C18 116.2(2) . . ?
C17 C16 C15 111.8(2) . . ?
C18 C16 C15 112.53(18) . . ?
C11 C19 C21 112.24(19) . . ?
C11 C19 C20 111.06(19) . . ?
C21 C19 C20 109.79(19) . . ?
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
Cl1 B1 1.757(3) . ?
Cl2 C2 1.6250(19) . ?
N1 C2 1.403(2) . ?
N1 B1 1.420(2) . ?
N1 C10 1.435(2) . ?
B1 N1 1.420(2) 8_575 ?
C2 C2 1.313(4) 8_575 ?
C10 C15 1.397(2) . ?
C10 C11 1.402(2) . ?
C11 C12 1.392(3) . ?
C11 C19 1.508(3) . ?
C12 C13 1.373(3) . ?
C13 C14 1.371(3) . ?
C14 C15 1.388(3) . ?
C15 C16 1.509(3) . ?
C16 C17 1.494(4) . ?
C16 C18 1.501(3) . ?
C19 C21 1.511(3) . ?
C19 C20 1.534(3) . ?
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
C2 N1 B1 N1 0.0(2) . . . 8_575 ?
C10 N1 B1 N1 170.43(11) . . . 8_575 ?
C2 N1 B1 Cl1 -179.05(16) . . . . ?
C10 N1 B1 Cl1 -8.7(3) . . . . ?
B1 N1 C2 C2 -0.02(14) . . . 8_575 ?
C10 N1 C2 C2 -171.37(11) . . . 8_575 ?
B1 N1 C2 Cl2 -178.29(16) . . . . ?
C10 N1 C2 Cl2 10.4(2) . . . . ?
C2 N1 C10 C15 -89.75(19) . . . . ?
B1 N1 C10 C15 101.2(2) . . . . ?
C2 N1 C10 C11 88.87(19) . . . . ?
B1 N1 C10 C11 -80.2(2) . . . . ?
C15 C10 C11 C12 -0.2(2) . . . . ?
N1 C10 C11 C12 -178.74(15) . . . . ?
C15 C10 C11 C19 -179.81(16) . . . . ?
N1 C10 C11 C19 1.6(2) . . . . ?
C10 C11 C12 C13 0.1(3) . . . . ?
C19 C11 C12 C13 179.71(18) . . . . ?
C11 C12 C13 C14 -0.2(3) . . . . ?
C12 C13 C14 C15 0.4(3) . . . . ?
C13 C14 C15 C10 -0.5(3) . . . . ?
C13 C14 C15 C16 179.41(18) . . . . ?
C11 C10 C15 C14 0.4(2) . . . . ?
N1 C10 C15 C14 178.94(15) . . . . ?
C11 C10 C15 C16 -179.52(16) . . . . ?
N1 C10 C15 C16 -1.0(2) . . . . ?
C14 C15 C16 C17 77.5(3) . . . . ?
C10 C15 C16 C17 -102.6(3) . . . . ?
C14 C15 C16 C18 -55.3(3) . . . . ?
C10 C15 C16 C18 124.6(2) . . . . ?
C12 C11 C19 C21 -65.0(2) . . . . ?
C10 C11 C19 C21 114.7(2) . . . . ?
C12 C11 C19 C20 58.4(3) . . . . ?
C10 C11 C19 C20 -122.0(2) . . . . ?
