#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:16:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179474 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/71/4337122.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_4337122
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_moiety         'C9 H10 B Be I N6'
_chemical_formula_sum            'C9 H10 B Be I N6'
_chemical_formula_weight         348.95
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.7981(11)
_cell_length_b                   14.2608(13)
_cell_length_c                   14.5214(13)
_cell_measurement_reflns_used    26633
_cell_measurement_temperature    180(1)
_cell_measurement_theta_max      32.67
_cell_measurement_theta_min      2.56
_cell_volume                     2650.3(4)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_computing_molecular_graphics    'BRUKER AXS SHELXTL Vers. 2008/4'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013/4)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013/4)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      180(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48086
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.721
_diffrn_reflns_theta_min         2.557
_diffrn_source                   'sealed X-RAY tube'
_exptl_absorpt_coefficient_mu    2.405
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.51
_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    1.749
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.280
_refine_diff_density_max         0.711
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         4822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0274P)²+1.6789P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4092
_reflns_number_total             4822
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic402895h_si_001.cif
_cod_data_source_block           dnp_024m_newlabl
_cod_database_code               4337122
#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   0.462
_shelx_estimated_absorpt_t_max   0.552
_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, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
I1 I 0.90220(2) 0.03761(2) 0.65538(2) 0.03551(4) Uani 1 1 d . .
Be1 Be 0.81991(14) 0.16014(12) 0.57784(13) 0.0221(3) Uani 1 1 d . .
B1 B 0.72731(14) 0.30696(13) 0.48816(13) 0.0295(3) Uani 1 1 d . .
H1 H 0.6962 0.3646 0.4460 0.035 Uiso 1 1 d R U
C13 C 0.55493(12) 0.27368(14) 0.58277(13) 0.0361(4) Uani 1 1 d . .
H13 H 0.5114 0.3223 0.5599 0.043 Uiso 1 1 d R U
N21 N 0.87841(10) 0.26798(9) 0.58753(8) 0.0234(2) Uani 1 1 d . .
C21 C 0.96268(12) 0.30802(12) 0.62526(11) 0.0295(3) Uani 1 1 d . .
H21 H 1.0128 0.2763 0.6622 0.035 Uiso 1 1 d R U
N22 N 0.82729(10) 0.33676(9) 0.54010(9) 0.0271(2) Uani 1 1 d . .
C22 C 0.96644(15) 0.40288(13) 0.60221(13) 0.0380(4) Uani 1 1 d . .
H22 H 1.0178 0.4474 0.6201 0.046 Uiso 1 1 d R U
N31 N 0.80651(9) 0.14974(9) 0.46018(9) 0.0237(2) Uani 1 1 d . .
C31 C 0.82353(12) 0.08860(12) 0.39223(11) 0.0307(3) Uani 1 1 d . .
H31 H 0.8551 0.0288 0.3996 0.037 Uiso 1 1 d R U
C33 C 0.74878(14) 0.21256(14) 0.33115(11) 0.0373(4) Uani 1 1 d . .
H33 H 0.7187 0.2558 0.2890 0.045 Uiso 1 1 d R U
C23 C 0.87953(15) 0.41797(12) 0.54870(13) 0.0350(3) Uani 1 1 d . .
H23 H 0.8600 0.4761 0.5217 0.042 Uiso 1 1 d R U
N32 N 0.76025(10) 0.22669(10) 0.42236(9) 0.0271(2) Uani 1 1 d . .
C32 C 0.78784(15) 0.12565(15) 0.30935(12) 0.0411(4) Uani 1 1 d . .
H32 H 0.7902 0.0968 0.2504 0.049 Uiso 1 1 d R U
N12 N 0.65531(9) 0.26036(9) 0.56023(10) 0.0272(2) Uani 1 1 d . .
C12 C 0.52555(13) 0.20566(15) 0.64464(12) 0.0388(4) Uani 1 1 d . .
H12 H 0.4590 0.1978 0.6726 0.047 Uiso 1 1 d R U
N11 N 0.69292(9) 0.18447(9) 0.60691(9) 0.0243(2) Uani 1 1 d . .
C11 C 0.61457(12) 0.15060(13) 0.65769(11) 0.0306(3) Uani 1 1 d . .
H11 H 0.6188 0.0971 0.6965 0.037 Uiso 1 1 d 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'
I I -0.4742 1.8119 '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
N11 Be1 N21 102.24(11)
N11 Be1 N31 99.62(11)
N21 Be1 N31 101.64(11)
N11 Be1 I1 117.46(10)
N21 Be1 I1 115.79(10)
N31 Be1 I1 117.35(10)
N12 B1 N22 106.36(13)
N12 B1 N32 105.20(13)
N22 B1 N32 106.20(12)
N12 C13 C12 108.79(16)
C21 N21 N22 106.64(13)
C21 N21 Be1 140.16(13)
N22 N21 Be1 113.16(11)
N21 C21 C22 110.10(15)
C23 N22 N21 109.51(14)
C23 N22 B1 134.02(14)
N21 N22 B1 116.46(12)
C23 C22 C21 105.05(15)
C31 N31 N32 107.40(13)
C31 N31 Be1 140.61(13)
N32 N31 Be1 111.93(11)
N31 C31 C32 109.75(16)
N32 C33 C32 108.77(16)
N22 C23 C22 108.70(16)
C33 N32 N31 108.85(14)
C33 N32 B1 133.38(15)
N31 N32 B1 117.68(12)
C33 C32 C31 105.23(15)
C13 N12 N11 109.24(14)
C13 N12 B1 132.60(15)
N11 N12 B1 117.86(12)
C13 C12 C11 105.21(14)
C11 N11 N12 107.24(13)
C11 N11 Be1 140.78(14)
N12 N11 Be1 111.87(11)
N11 C11 C12 109.53(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
I1 Be1 2.3303(18)
Be1 N11 1.715(2)
Be1 N21 1.716(2)
Be1 N31 1.724(2)
B1 N12 1.545(2)
B1 N22 1.545(2)
B1 N32 1.550(2)
C13 N12 1.339(2)
C13 C12 1.375(3)
N21 C21 1.3376(19)
N21 N22 1.3655(17)
C21 C22 1.394(2)
N22 C23 1.343(2)
C22 C23 1.374(3)
N31 C31 1.3347(19)
N31 N32 1.3625(17)
C31 C32 1.391(3)
C33 N32 1.348(2)
C33 C32 1.374(3)
N12 N11 1.3648(18)
C12 C11 1.397(3)
N11 C11 1.3351(19)
