#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:07:58 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180004 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/98/7029830.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_7029830
loop_
_publ_author_name
'Nitschke, Christian'
'Köckerling, Martin'
'Bernhardt, Eduard'
'Küppers, Torsten'
'Willner, Helge'
_publ_section_title
;
 Structural diversity and spectral and thermal properties of the first
 alkaline earth metal tetracyanidoborates: [Mg(H2O)6][B(CN)4]2,
 [Mg(H2O)2][B(CN)4]2, [Mg(DMF)6][B(CN)4]2, [Ca(H2O)3][B(CN)4]2, and
 [Ca(H2O)2(CH3CN)][B(CN)4]2.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7128
_journal_page_last               7138
_journal_paper_doi               10.1039/c3dt51945g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         '(Ca 2+), (C4 N4 B -1)2, (C2 H3 N), 2(H2 O)'
_chemical_formula_sum            'C10 H7 B2 Ca N9 O2'
_chemical_formula_weight         346.95
_chemical_name_systematic
;
Calcium bis-aqua bis-tetracyanoborate acetronitrile solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'ct.exe (M. Köckerling, 1996)'
_cell_angle_alpha                90.00
_cell_angle_beta                 116.538(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2203(2)
_cell_length_b                   12.6637(2)
_cell_length_c                   13.5191(2)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      35.96
_cell_measurement_theta_min      3.04
_cell_volume                     1871.71(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37481
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.51
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_correction_T_min  0.9164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker-Nonius SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         8728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0490P)²+0.1313P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                6825
_reflns_number_total             8728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51945g1.cif
_cod_data_source_block           Ca_BCN_Aceto
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-12899/cifs/7029830.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7029830
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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
Ca1 Ca 0.221247(13) 0.483452(11) 0.834516(11) 0.01858(4) Uani 1 1 d .
B1 B -0.03413(8) 0.25157(7) 0.98462(7) 0.02084(14) Uani 1 1 d .
N1 N 0.09999(7) 0.35543(7) 0.89831(6) 0.03255(16) Uani 1 1 d .
C1 C 0.04418(8) 0.31150(6) 0.93422(6) 0.02488(14) Uani 1 1 d .
N2 N 0.11664(8) 0.14397(7) 1.17146(7) 0.03658(18) Uani 1 1 d .
C2 C 0.05497(8) 0.18960(7) 1.09352(7) 0.02680(15) Uani 1 1 d .
N3 N -0.16067(8) 0.39632(6) 1.04339(7) 0.03412(16) Uani 1 1 d .
C3 C -0.11006(8) 0.33577(6) 1.01644(6) 0.02480(14) Uani 1 1 d .
N4 N -0.18074(8) 0.10955(7) 0.82988(7) 0.03833(18) Uani 1 1 d .
C4 C -0.12282(8) 0.16965(7) 0.89549(7) 0.02650(15) Uani 1 1 d .
B2 B -0.25898(9) 0.52285(8) 0.63382(8) 0.02745(17) Uani 1 1 d .
N5 N -0.00975(8) 0.52944(8) 0.73141(7) 0.03878(19) Uani 1 1 d .
C5 C -0.11397(9) 0.52839(7) 0.68962(8) 0.03182(17) Uani 1 1 d .
N6 N -0.33428(12) 0.32741(8) 0.54458(11) 0.0592(3) Uani 1 1 d .
C6 C -0.30292(10) 0.40995(8) 0.57928(9) 0.03685(19) Uani 1 1 d .
N7 N -0.33570(13) 0.54661(12) 0.79336(11) 0.0658(3) Uani 1 1 d .
C7 C -0.30389(11) 0.53839(10) 0.72632(9) 0.0415(2) Uani 1 1 d .
N8 N -0.35172(11) 0.68157(8) 0.48286(9) 0.0556(3) Uani 1 1 d .
C8 C -0.31416(9) 0.61386(7) 0.54417(8) 0.03370(18) Uani 1 1 d .
N9 N 0.38856(9) 0.39287(8) 0.80496(7) 0.0435(2) Uani 1 1 d .
C9 C 0.46043(9) 0.34375(9) 0.79461(7) 0.0356(2) Uani 1 1 d .
C10 C 0.55341(11) 0.28067(11) 0.78278(10) 0.0469(3) Uani 1 1 d .
H10A H 0.6330 0.2967 0.8428 0.070 Uiso 1 1 calc R
H10B H 0.5536 0.2969 0.7127 0.070 Uiso 1 1 calc R
H10C H 0.5356 0.2063 0.7849 0.070 Uiso 1 1 calc R
O1 O 0.37958(7) 0.61012(6) 0.91291(7) 0.03687(15) Uani 1 1 d .
H1 H 0.3667(15) 0.6727(13) 0.9275(13) 0.061(4) Uiso 1 1 d .
H2 H 0.4597(16) 0.6006(12) 0.9377(13) 0.058(4) Uiso 1 1 d .
O2 O 0.36390(6) 0.40646(5) 1.01410(5) 0.02702(12) Uani 1 1 d .
H3 H 0.3506(14) 0.4295(13) 1.0655(14) 0.063(5) Uiso 1 1 d .
H4 H 0.3508(14) 0.3394(13) 1.0160(13) 0.062(5) 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
O1 Ca1 O2 75.57(3) . .
O1 Ca1 N9 79.70(3) . .
O2 Ca1 N9 73.18(3) . .
O1 Ca1 N2 143.57(3) . 4_565
O2 Ca1 N2 117.27(3) . 4_565
N9 Ca1 N2 72.92(3) . 4_565
O1 Ca1 N3 74.04(3) . 3_567
O2 Ca1 N3 83.26(3) . 3_567
N9 Ca1 N3 148.33(3) . 3_567
N2 Ca1 N3 138.10(3) 4_565 3_567
O1 Ca1 N1 138.55(3) . .
O2 Ca1 N1 71.53(2) . .
N9 Ca1 N1 113.09(3) . .
N2 Ca1 N1 75.69(3) 4_565 .
N3 Ca1 N1 77.67(3) 3_567 .
O1 Ca1 N5 124.30(3) . .
O2 Ca1 N5 137.48(3) . .
N9 Ca1 N5 141.24(3) . .
N2 Ca1 N5 71.02(3) 4_565 .
N3 Ca1 N5 69.98(3) 3_567 .
N1 Ca1 N5 70.88(3) . .
O1 Ca1 N4 76.81(3) . 2_556
O2 Ca1 N4 149.81(3) . 2_556
N9 Ca1 N4 90.12(3) . 2_556
N2 Ca1 N4 79.64(3) 4_565 2_556
N3 Ca1 N4 100.64(3) 3_567 2_556
N1 Ca1 N4 138.65(3) . 2_556
N5 Ca1 N4 69.93(3) . 2_556
C4 B1 C2 109.37(7) . .
C4 B1 C1 108.81(6) . .
C2 B1 C1 109.69(7) . .
C4 B1 C3 111.02(7) . .
C2 B1 C3 108.68(6) . .
C1 B1 C3 109.27(6) . .
C1 N1 Ca1 170.00(8) . .
N1 C1 B1 179.32(9) . .
C2 N2 Ca1 169.09(8) . 4_566
N2 C2 B1 178.48(9) . .
C3 N3 Ca1 161.70(8) . 3_567
N3 C3 B1 177.26(9) . .
C4 N4 Ca1 152.68(8) . 2_546
N4 C4 B1 175.78(9) . .
C7 B2 C5 109.01(8) . .
C7 B2 C8 109.45(8) . .
C5 B2 C8 109.50(8) . .
C7 B2 C6 108.26(8) . .
C5 B2 C6 109.55(8) . .
C8 B2 C6 111.03(8) . .
C5 N5 Ca1 166.00(8) . .
N5 C5 B2 177.81(10) . .
N6 C6 B2 176.88(12) . .
N7 C7 B2 178.09(13) . .
N8 C8 B2 177.59(11) . .
C9 N9 Ca1 173.61(10) . .
N9 C9 C10 179.31(11) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
Ca1 O1 H1 122.6(11) . .
Ca1 O1 H2 128.1(10) . .
H1 O1 H2 109.0(14) . .
Ca1 O2 H3 111.5(11) . .
Ca1 O2 H4 110.9(11) . .
H3 O2 H4 102.1(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O1 2.3680(7) .
Ca1 O2 2.4702(6) .
Ca1 N9 2.5271(9) .
Ca1 N2 2.5650(8) 4_565
Ca1 N3 2.5849(8) 3_567
Ca1 N1 2.5904(8) .
Ca1 N5 2.5951(9) .
Ca1 N4 2.5983(8) 2_556
B1 C4 1.5924(12) .
B1 C2 1.5926(12) .
B1 C1 1.5935(12) .
B1 C3 1.5937(11) .
N1 C1 1.1428(11) .
N2 C2 1.1413(11) .
N2 Ca1 2.5650(8) 4_566
N3 C3 1.1422(11) .
N3 Ca1 2.5849(8) 3_567
N4 C4 1.1428(11) .
N4 Ca1 2.5983(8) 2_546
B2 C7 1.5865(15) .
B2 C5 1.5874(14) .
B2 C8 1.5880(13) .
B2 C6 1.5881(14) .
N5 C5 1.1395(13) .
N6 C6 1.1397(14) .
N7 C7 1.1394(15) .
N8 C8 1.1371(13) .
N9 C9 1.1347(12) .
C9 C10 1.4551(14) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C10 H10C 0.9700 .
O1 H1 0.848(17) .
O1 H2 0.890(17) .
O2 H3 0.834(17) .
O2 H4 0.866(17) .
