#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:16:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179474 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/71/4337119.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_4337119
loop_
_publ_author_name
'Naglav, Dominik'
'Bläser, Dieter'
'Wölper, Christoph'
'Schulz, Stephan'
_publ_contact_author
;
         Prof. Dr. Schulz, Stephan
         Fachbereich Chemie der
         Universität Duisburg-Essen
         Campus Essen, Universitätsstr. 7
         D-45141 Essen, Germany
;
_publ_section_title
;
 Synthesis and Characterization of Heteroleptic 1-Tris(pyrazolyl)borate
 Beryllium Complexes.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1241
_journal_page_last               1249
_journal_paper_doi               10.1021/ic402895h
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C9 H10 B Be Cl N6'
_chemical_formula_weight         257.50
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.740(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6712(5)
_cell_length_b                   12.6310(9)
_cell_length_c                   12.9757(8)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      2.89
_cell_volume                     1239.16(14)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18765
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.533
_diffrn_reflns_theta_min         2.266
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0416P)²+0.4319P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3214
_reflns_number_total             3743
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic402895h_si_001.cif
_cod_data_source_block           dnd_001m_newlabl
_cod_database_code               4337119
#BEGIN Tags that were not found in dictionaries:
_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   0.924
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
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 0.26517(4) 0.60189(2) 0.51945(2) 0.02445(8) Uani 1 1 d . .
B1 B 0.21287(14) 0.75208(9) 0.18472(8) 0.01558(19) Uani 1 1 d . .
H1 H 0.2010 0.7834 0.1131 0.019 Uiso 1 1 calc R U
Be1 Be 0.24691(16) 0.66570(10) 0.38281(9) 0.0149(2) Uani 1 1 d . .
N11 N 0.43800(10) 0.68269(7) 0.33031(6) 0.01510(16) Uani 1 1 d . .
N12 N 0.40722(11) 0.72749(7) 0.23334(6) 0.01513(16) Uani 1 1 d . .
N21 N 0.11592(11) 0.59965(6) 0.28153(7) 0.01518(16) Uani 1 1 d . .
N22 N 0.10988(11) 0.64675(7) 0.18656(6) 0.01594(16) Uani 1 1 d . .
N31 N 0.15894(10) 0.79209(7) 0.36476(6) 0.01470(16) Uani 1 1 d . .
N32 N 0.14279(10) 0.82626(6) 0.26379(6) 0.01444(15) Uani 1 1 d . .
C11 C 0.61333(13) 0.67248(8) 0.35759(8) 0.0196(2) Uani 1 1 d . .
H11 H 0.6719 0.6431 0.4215 0.023 Uiso 1 1 calc R U
C12 C 0.69723(13) 0.71153(9) 0.27807(9) 0.0231(2) Uani 1 1 d . .
H12 H 0.8207 0.7140 0.2771 0.028 Uiso 1 1 calc R U
C13 C 0.56186(13) 0.74579(8) 0.20100(8) 0.0196(2) Uani 1 1 d . .
H13 H 0.5759 0.7769 0.1363 0.023 Uiso 1 1 calc R U
C21 C 0.01591(13) 0.51278(8) 0.26654(9) 0.0211(2) Uani 1 1 d . .
H21 H -0.0039 0.4651 0.3200 0.025 Uiso 1 1 calc R U
C22 C -0.05514(14) 0.50237(9) 0.16095(10) 0.0264(2) Uani 1 1 d . .
H22 H -0.1302 0.4476 0.1288 0.032 Uiso 1 1 calc R U
C23 C 0.00703(14) 0.58889(9) 0.11288(9) 0.0227(2) Uani 1 1 d . .
H23 H -0.0184 0.6048 0.0403 0.027 Uiso 1 1 calc R U
C31 C 0.09524(13) 0.86941(8) 0.41845(8) 0.01952(19) Uani 1 1 d . .
H31 H 0.0902 0.8671 0.4911 0.023 Uiso 1 1 calc R U
C32 C 0.03729(14) 0.95393(8) 0.35190(9) 0.0224(2) Uani 1 1 d . .
H32 H -0.0135 1.0186 0.3696 0.027 Uiso 1 1 calc R U
C33 C 0.06983(13) 0.92294(8) 0.25471(9) 0.01862(19) Uani 1 1 d . .
H33 H 0.0447 0.9633 0.1922 0.022 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'
Be Be 0.0005 0.0002 '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
N12 B1 N22 106.24(8)
N12 B1 N32 105.61(8)
N22 B1 N32 105.89(7)
N21 Be1 N11 100.53(7)
N21 Be1 N31 100.30(7)
N11 Be1 N31 99.72(7)
N21 Be1 Cl1 116.06(7)
N11 Be1 Cl1 118.58(7)
N31 Be1 Cl1 118.32(7)
C11 N11 N12 107.07(8)
C11 N11 Be1 139.84(9)
N12 N11 Be1 112.87(7)
C13 N12 N11 109.60(8)
C13 N12 B1 132.70(9)
N11 N12 B1 117.62(7)
C21 N21 N22 107.26(8)
C21 N21 Be1 138.94(9)
N22 N21 Be1 113.80(7)
C23 N22 N21 109.35(9)
C23 N22 B1 133.92(9)
N21 N22 B1 116.71(8)
C31 N31 N32 106.67(8)
C31 N31 Be1 140.30(8)
N32 N31 Be1 113.01(7)
C33 N32 N31 109.95(8)
C33 N32 B1 132.73(8)
N31 N32 B1 117.29(8)
N11 C11 C12 109.82(9)
C13 C12 C11 105.15(9)
N12 C13 C12 108.36(9)
N21 C21 C22 109.92(10)
C23 C22 C21 105.17(9)
N22 C23 C22 108.30(10)
N31 C31 C32 109.97(9)
C33 C32 C31 105.05(9)
N32 C33 C32 108.35(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cl1 Be1 1.9310(12)
B1 N12 1.5489(13)
B1 N22 1.5496(14)
B1 N32 1.5512(13)
Be1 N21 1.7279(15)
Be1 N11 1.7312(14)
Be1 N31 1.7337(15)
N11 C11 1.3378(12)
N11 N12 1.3633(11)
N12 C13 1.3435(12)
N21 C21 1.3342(13)
N21 N22 1.3621(12)
N22 C23 1.3473(13)
N31 C31 1.3390(12)
N31 N32 1.3651(11)
N32 C33 1.3401(12)
C11 C12 1.3953(16)
C12 C13 1.3835(16)
C21 C22 1.3925(16)
C22 C23 1.3826(17)
C31 C32 1.3976(15)
C32 C33 1.3829(15)
