#------------------------------------------------------------------------------
#$Date: 2016-03-24 02:04:06 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179554 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/23/4502369.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_4502369
loop_
_publ_author_name
'Paul, Avijit Kumar'
'Sachidananda, K.'
'Natarajan, Srinivasan'
_publ_section_title
;
 [B4O9H2] Cyclic Borate Units as the Building Unit in a Family of Zinc
 Borate Structures
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              456
_journal_paper_doi               10.1021/cg901054h
_journal_volume                  10
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_sum            'C3 H12 B4 N2 O8 Zn'
_chemical_formula_weight         312.76
_chemical_name_common            ‘Zinc-Borate’
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0474(3)
_cell_length_b                   7.8332(3)
_cell_length_c                   19.2197(7)
_cell_measurement_reflns_used    2012
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.59
_cell_volume                     1061.00(7)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'Ortep-3 for windows (Farrugia, 1999) and CAMERON (Watkin et al., 1993)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6196
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    2.348
_exptl_absorpt_correction_T_max  0.9119
_exptl_absorpt_correction_T_min  0.7659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.575
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0682P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                1874
_reflns_number_total             2012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg901054h_si_001.cif
_cod_data_source_block           Compound(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4502369
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.31739(7) 0.95343(6) 0.82559(3) 0.01589(16) Uani 1 1 d .
O1 O 0.4597(4) 0.7455(3) 0.83690(14) 0.0138(6) Uani 1 1 d .
O2 O 0.4473(4) 1.0115(4) 0.73587(15) 0.0164(6) Uani 1 1 d .
O3 O 0.6773(5) 0.7854(3) 0.73860(14) 0.0168(6) Uani 1 1 d .
O4 O 0.2474(5) 0.6897(4) 0.93233(16) 0.0202(7) Uani 1 1 d .
H4 H 0.2812 0.7795 0.9504 0.030 Uiso 1 1 calc R
O5 O 0.7822(4) 0.6487(4) 0.84132(15) 0.0172(6) Uani 1 1 d .
O6 O 0.6653(5) 0.9646(3) 0.64345(15) 0.0198(7) Uani 1 1 d .
O7 O 0.5700(5) 0.5828(4) 0.93490(16) 0.0221(7) Uani 1 1 d .
O8 O 0.8938(5) 0.5840(5) 0.95631(16) 0.0245(8) Uani 1 1 d .
H8 H 0.9951 0.5991 0.9363 0.037 Uiso 1 1 calc R
N1 N 0.2916(6) 1.1084(5) 0.9108(2) 0.0200(9) Uani 1 1 d .
H1A H 0.3374 1.0927 0.8698 0.024 Uiso 1 1 calc R
H1B H 0.3657 1.1086 0.9464 0.024 Uiso 1 1 calc R
N2 N 0.0310(6) 0.9772(6) 0.8135(2) 0.0334(10) Uani 1 1 d .
H2A H 0.1131 0.9070 0.8301 0.040 Uiso 1 1 calc R
H2B H -0.0202 0.9579 0.7736 0.040 Uiso 1 1 calc R
B1 B 0.6192(7) 0.6807(6) 0.7967(2) 0.0132(9) Uani 1 1 d .
B2 B 0.5967(7) 0.9206(6) 0.7059(2) 0.0136(9) Uani 1 1 d .
B3 B 0.4018(8) 0.6194(6) 0.8926(2) 0.0142(10) Uani 1 1 d .
B4 B 0.7456(8) 0.6038(6) 0.9093(3) 0.0156(10) Uani 1 1 d .
C1 C 0.0855(9) 1.1350(9) 0.9202(3) 0.0440(16) Uani 1 1 d .
H1C H 0.0650 1.2444 0.9426 0.053 Uiso 1 1 calc R
H1D H 0.0363 1.0471 0.9508 0.053 Uiso 1 1 calc R
C2 C -0.0223(10) 1.1309(9) 0.8534(4) 0.0492(16) Uani 1 1 d .
H2 H 0.0076 1.2331 0.8261 0.059 Uiso 1 1 calc R
C3 C -0.2365(9) 1.1290(11) 0.8708(5) 0.079(3) Uani 1 1 d .
H3A H -0.3086 1.1266 0.8284 0.118 Uiso 1 1 calc R
H3B H -0.2685 1.2296 0.8968 0.118 Uiso 1 1 calc R
H3C H -0.2655 1.0295 0.8979 0.118 Uiso 1 1 calc R
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
O1 Zn1 O2 92.95(12) . .
O1 Zn1 N2 127.25(16) . .
O2 Zn1 N2 109.45(17) . .
O1 Zn1 N1 117.23(14) . .
O2 Zn1 N1 126.47(14) . .
N2 Zn1 N1 87.10(17) . .
B1 O1 B3 110.9(3) . .
B1 O1 Zn1 129.6(2) . .
B3 O1 Zn1 119.5(3) . .
B2 O2 B1 120.1(3) . 4_656
B2 O2 Zn1 125.7(3) . .
B1 O2 Zn1 114.0(2) 4_656 .
B2 O3 B1 133.1(4) . .
B3 O4 H4 109.5 . .
B4 O5 B1 117.1(4) . .
B2 O6 B3 121.1(4) . 4_656
B4 O7 B3 121.2(3) . .
B4 O8 H8 109.5 . .
C1 N1 Zn1 105.6(4) . .
C1 N1 H1A 120.0 . .
Zn1 N1 H1A 31.7 . .
C1 N1 H1B 120.0 . .
Zn1 N1 H1B 125.7 . .
H1A N1 H1B 120.0 . .
C2 N2 Zn1 105.4(4) . .
C2 N2 H2A 120.0 . .
Zn1 N2 H2A 39.9 . .
C2 N2 H2B 120.0 . .
Zn1 N2 H2B 120.0 . .
H2A N2 H2B 120.0 . .
O3 B1 O5 109.2(4) . .
O3 B1 O1 115.5(3) . .
O5 B1 O1 110.9(3) . .
O3 B1 O2 105.1(3) . 4_646
O5 B1 O2 109.4(3) . 4_646
O1 B1 O2 106.3(3) . 4_646
O6 B2 O3 117.7(4) . .
O6 B2 O2 120.8(4) . .
O3 B2 O2 121.5(4) . .
O4 B3 O7 113.0(3) . .
O4 B3 O6 108.7(4) . 4_646
O7 B3 O6 111.1(4) . 4_646
O4 B3 O1 109.3(3) . .
O7 B3 O1 107.6(4) . .
O6 B3 O1 107.0(3) 4_646 .
O7 B4 O5 123.5(4) . .
O7 B4 O8 116.2(4) . .
O5 B4 O8 120.3(4) . .
N1 C1 C2 113.1(5) . .
N1 C1 H1C 109.0 . .
C2 C1 H1C 109.0 . .
N1 C1 H1D 109.0 . .
C2 C1 H1D 109.0 . .
H1C C1 H1D 107.8 . .
N2 C2 C1 109.6(5) . .
N2 C2 C3 110.6(6) . .
C1 C2 C3 108.2(6) . .
N2 C2 H2 109.5 . .
C1 C2 H2 109.5 . .
C3 C2 H2 109.5 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 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
Zn1 O1 1.925(3) .
Zn1 O2 2.005(3) .
Zn1 N2 2.041(4) .
Zn1 N1 2.047(4) .
O1 B1 1.455(6) .
O1 B3 1.512(5) .
O2 B2 1.396(6) .
O2 B1 1.539(5) 4_656
O3 B2 1.357(6) .
O3 B1 1.445(5) .
O4 B3 1.439(6) .
O4 H4 0.8200 .
O5 B4 1.378(6) .
O5 B1 1.455(6) .
O6 B2 1.339(6) .
O6 B3 1.474(6) 4_656
O7 B4 1.342(7) .
O7 B3 1.466(6) .
O8 B4 1.389(6) .
O8 H8 0.8200 .
N1 C1 1.478(7) .
N1 H1A 0.8600 .
N1 H1B 0.8600 .
N2 C2 1.477(8) .
N2 H2A 0.8600 .
N2 H2B 0.8600 .
B1 O2 1.539(5) 4_646
B3 O6 1.474(6) 4_646
C1 C2 1.491(9) .
C1 H1C 0.9700 .
C1 H1D 0.9700 .
C2 C3 1.547(10) .
C2 H2 0.9800 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
