#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:38:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179196 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/35/4313561.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_4313561
loop_
_publ_author_name
'Barton H. Hamilton'
'Kathryn A. Kelly'
'Wilhelm Malasi'
'Christopher J. Ziegler'
_publ_section_title
;
 Tetrakis(imidazolyl)borate-Based Coordination Polymers: Group II Network
 Solids, M[B(Im)4]2(H2O)2 (M = Mg, Ca, Sr)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3067
_journal_page_last               3073
_journal_paper_doi               10.1021/ic026244x
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C24 H28 B2 Ca N16 O2'
_chemical_formula_weight         634.32
_chemical_name_common            'Calcium tetrakis(imidazolyl)borate'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.39(3)
_cell_angle_beta                 108.36(3)
_cell_angle_gamma                118.04(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3893(19)
_cell_length_b                   9.6820(19)
_cell_length_c                   10.384(2)
_cell_measurement_reflns_used    3239
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.13
_cell_volume                     766.2(4)
_computing_cell_refinement       P3
_computing_data_collection       P3
_computing_data_reduction        xdisk
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P(2)1 Syntex'
_diffrn_measurement_method       '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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3239
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.13
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  3/97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         2701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0340
_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)+(0.0188P)²+0.4498P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0702
_reflns_number_gt                2229
_reflns_number_total             2701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026244xsi20021206_024518_3.cif
_cod_data_source_block           Ca[B(Im)4].2H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        766.2(3)
_cod_database_code               4313561
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.5000 0.5000 0.5000 0.01190(14) Uani 1 2 d S . .
B1 B 0.2333(3) -0.1269(2) 0.1506(2) 0.0137(4) Uani 1 1 d . . .
O1 O 0.78800(18) 0.63891(17) 0.51869(15) 0.0207(3) Uani 1 1 d . . .
H14 H 0.888(4) 0.677(3) 0.594(3) 0.054(8) Uiso 1 1 d . . .
H13 H 0.818(3) 0.674(3) 0.449(3) 0.051(8) Uiso 1 1 d . . .
N7 N 0.5236(2) 0.29964(18) 0.63145(15) 0.0166(3) Uani 1 1 d . . .
N4 N -0.1026(2) -0.25383(19) 0.30565(16) 0.0187(4) Uani 1 1 d . . .
N8 N 0.63356(19) 0.16188(17) 0.74860(15) 0.0130(3) Uani 1 1 d . . .
N1 N 0.4010(2) 0.30701(18) 0.27921(16) 0.0170(3) Uani 1 1 d . . .
N6 N 0.0797(2) -0.25454(19) -0.23706(16) 0.0198(4) Uani 1 1 d . . .
N2 N 0.31184(19) 0.05738(17) 0.17289(15) 0.0122(3) Uani 1 1 d . . .
N5 N 0.18843(19) -0.20023(17) -0.00260(15) 0.0137(3) Uani 1 1 d . . .
N3 N 0.06599(19) -0.19942(17) 0.18256(15) 0.0132(3) Uani 1 1 d . . .
C9 C 0.1820(2) -0.3395(2) -0.0526(2) 0.0172(4) Uani 1 1 d . . .
H9 H 0.220(3) -0.395(2) 0.009(2) 0.022(5) Uiso 1 1 d . . .
C1 C 0.2963(2) 0.1509(2) 0.26237(18) 0.0147(4) Uani 1 1 d . . .
H1 H 0.215(3) 0.107(2) 0.309(2) 0.018(5) Uiso 1 1 d . . .
C2 C 0.4912(2) 0.3142(2) 0.19468(19) 0.0170(4) Uani 1 1 d . . .
H2 H 0.575(3) 0.413(3) 0.189(2) 0.020(5) Uiso 1 1 d . . .
C8 C 0.1168(2) -0.3701(2) -0.1944(2) 0.0193(4) Uani 1 1 d . . .
H8 H 0.098(3) -0.454(3) -0.260(2) 0.022(5) Uiso 1 1 d . . .
C10 C 0.6666(2) 0.2999(2) 0.70614(19) 0.0167(4) Uani 1 1 d . . .
H10 H 0.785(3) 0.385(2) 0.730(2) 0.019(5) Uiso 1 1 d . . .
C4 C 0.0558(2) -0.2074(2) 0.30977(19) 0.0153(4) Uani 1 1 d . . .
H4 H 0.152(2) -0.185(2) 0.390(2) 0.013(5) Uiso 1 1 d . . .
C11 C 0.3883(3) 0.1516(2) 0.6265(2) 0.0175(4) Uani 1 1 d . . .
H11 H 0.269(3) 0.122(2) 0.580(2) 0.021(5) Uiso 1 1 d . . .
C7 C 0.1241(2) -0.1564(2) -0.11921(19) 0.0176(4) Uani 1 1 d . . .
H7 H 0.115(2) -0.061(2) -0.1144(19) 0.016(5) Uiso 1 1 d . . .
C5 C -0.2002(3) -0.2751(2) 0.1667(2) 0.0184(4) Uani 1 1 d . . .
H5 H -0.322(3) -0.308(2) 0.134(2) 0.023(5) Uiso 1 1 d . . .
C3 C 0.4385(2) 0.1636(2) 0.12988(19) 0.0155(4) Uani 1 1 d . . .
H3 H 0.474(2) 0.125(2) 0.065(2) 0.015(5) Uiso 1 1 d . . .
C12 C 0.4531(2) 0.0675(2) 0.69703(19) 0.0162(4) Uani 1 1 d . . .
H12 H 0.398(3) -0.037(3) 0.715(2) 0.025(6) Uiso 1 1 d . . .
C6 C -0.1002(2) -0.2428(2) 0.0908(2) 0.0158(4) Uani 1 1 d . . .
H6 H -0.126(3) -0.247(2) -0.006(2) 0.024(6) Uiso 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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
O1 Ca1 O1 180.0 . 2_666 ?
O1 Ca1 N1 87.05(7) . 2_666 ?
O1 Ca1 N1 92.95(7) 2_666 2_666 ?
O1 Ca1 N1 92.95(7) . . ?
O1 Ca1 N1 87.05(7) 2_666 . ?
N1 Ca1 N1 180.0 2_666 . ?
O1 Ca1 N7 96.77(6) . . ?
O1 Ca1 N7 83.23(6) 2_666 . ?
N1 Ca1 N7 90.78(5) 2_666 . ?
N1 Ca1 N7 89.22(5) . . ?
O1 Ca1 N7 83.23(6) . 2_666 ?
O1 Ca1 N7 96.77(6) 2_666 2_666 ?
N1 Ca1 N7 89.22(5) 2_666 2_666 ?
N1 Ca1 N7 90.78(5) . 2_666 ?
N7 Ca1 N7 180.0 . 2_666 ?
N5 B1 N8 110.25(15) . 2_656 ?
N5 B1 N2 108.81(15) . . ?
N8 B1 N2 109.85(15) 2_656 . ?
N5 B1 N3 110.30(15) . . ?
N8 B1 N3 109.04(14) 2_656 . ?
N2 B1 N3 108.57(15) . . ?
C10 N7 C11 104.13(16) . . ?
C10 N7 Ca1 128.18(13) . . ?
C11 N7 Ca1 127.16(12) . . ?
C4 N4 C5 104.32(16) . . ?
C10 N8 C12 104.75(15) . . ?
C10 N8 B1 127.67(15) . 2_656 ?
C12 N8 B1 127.08(15) . 2_656 ?
C1 N1 C2 104.39(15) . . ?
C1 N1 Ca1 119.88(12) . . ?
C2 N1 Ca1 128.61(12) . . ?
C7 N6 C8 104.27(16) . . ?
C1 N2 C3 105.40(15) . . ?
C1 N2 B1 125.75(15) . . ?
C3 N2 B1 127.64(15) . . ?
C7 N5 C9 104.85(16) . . ?
C7 N5 B1 127.89(15) . . ?
C9 N5 B1 126.71(16) . . ?
C4 N3 C6 105.51(15) . . ?
C4 N3 B1 127.35(15) . . ?
C6 N3 B1 126.24(15) . . ?
C8 C9 N5 107.11(17) . . ?
N1 C1 N2 113.18(16) . . ?
C3 C2 N1 109.96(17) . . ?
C9 C8 N6 110.31(17) . . ?
N7 C10 N8 113.56(17) . . ?
N4 C4 N3 112.90(17) . . ?
C12 C11 N7 110.12(17) . . ?
N6 C7 N5 113.46(17) . . ?
C6 C5 N4 110.51(17) . . ?
C2 C3 N2 107.08(17) . . ?
C11 C12 N8 107.44(17) . . ?
C5 C6 N3 106.75(17) . . ?
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
Ca1 O1 2.3190(16) . ?
Ca1 O1 2.3190(16) 2_666 ?
Ca1 N1 2.4760(19) 2_666 ?
Ca1 N1 2.4760(19) . ?
Ca1 N7 2.4904(16) . ?
Ca1 N7 2.4904(16) 2_666 ?
B1 N5 1.541(3) . ?
B1 N8 1.545(2) 2_656 ?
B1 N2 1.546(2) . ?
B1 N3 1.546(3) . ?
N7 C10 1.321(2) . ?
N7 C11 1.382(2) . ?
N4 C4 1.321(2) . ?
N4 C5 1.385(2) . ?
N8 C10 1.357(2) . ?
N8 C12 1.381(2) . ?
N8 B1 1.545(2) 2_656 ?
N1 C1 1.321(2) . ?
N1 C2 1.383(2) . ?
N6 C7 1.320(2) . ?
N6 C8 1.378(3) . ?
N2 C1 1.348(2) . ?
N2 C3 1.382(2) . ?
N5 C7 1.361(2) . ?
N5 C9 1.382(2) . ?
N3 C4 1.358(2) . ?
N3 C6 1.386(2) . ?
C9 C8 1.356(3) . ?
C2 C3 1.349(3) . ?
C11 C12 1.351(3) . ?
C5 C6 1.349(3) . ?
