#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:06:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179362 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/59/4325981.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_4325981
loop_
_publ_author_name
'Mark J. Saly'
'Jing Li'
'Mary Jane Heeg'
'Charles H. Winter'
_publ_section_title
;
 Efficient Hydride and Pyrazolyl Redistribution upon Thermolysis of a
 Calcium Complex Containing Dihydrobis(pyrazolyl)borate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7385
_journal_page_last               7387
_journal_paper_doi               10.1021/ic2012815
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C47 H81 B7 Ca3 N18 O13'
_chemical_formula_weight         1302.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.9880(4)
_cell_length_b                   16.9880(4)
_cell_length_c                   13.5711(4)
_cell_measurement_reflns_used    5312
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      2.4
_cell_volume                     3391.80(15)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       'Bruker APEX2'
_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  0.0904
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40352
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.9695
_exptl_absorpt_correction_T_min  0.9318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       rods
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0506P)²+0.7758P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                2074
_reflns_number_total             2920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2012815_si_002_4.cif
_cod_data_source_block           bcat
_cod_database_code               4325981
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.43542(3) 0.23197(3) 0.7500 0.01880(13) Uani 1 2 d S . .
N1 N 0.32110(9) 0.13079(10) 0.62915(11) 0.0234(3) Uani 1 1 d . . .
N2 N 0.23163(9) 0.08704(9) 0.65621(11) 0.0231(3) Uani 1 1 d . . .
C1 C 0.32372(13) 0.09271(12) 0.54437(14) 0.0282(4) Uani 1 1 d . . .
H1 H 0.3777 0.1102 0.5079 0.034 Uiso 1 1 calc R . .
C2 C 0.23819(13) 0.02454(12) 0.51580(14) 0.0314(4) Uani 1 1 d . . .
H2 H 0.2224 -0.0128 0.4588 0.038 Uiso 1 1 calc R . .
C3 C 0.18181(12) 0.02334(12) 0.58821(14) 0.0287(4) Uani 1 1 d . . .
H3 H 0.1178 -0.0160 0.5904 0.034 Uiso 1 1 calc R . .
N3 N 0.31872(13) 0.27718(13) 0.7500 0.0277(5) Uani 1 2 d S . .
N4 N 0.22844(13) 0.21332(13) 0.7500 0.0228(4) Uani 1 2 d S . .
C4 C 0.32196(18) 0.35639(18) 0.7500 0.0402(8) Uani 1 2 d S . .
H4 H 0.3766 0.4135 0.7500 0.048 Uiso 1 2 calc SR . .
C5 C 0.2359(2) 0.3461(2) 0.7500 0.0466(9) Uani 1 2 d S . .
H5 H 0.2204 0.3926 0.7500 0.056 Uiso 1 2 calc SR . .
C6 C 0.17837(18) 0.2546(2) 0.7500 0.0346(6) Uani 1 2 d S . .
H6 H 0.1139 0.2249 0.7500 0.041 Uiso 1 2 calc SR . .
B1 B 0.19673(19) 0.11123(19) 0.7500 0.0254(6) Uani 1 2 d S . .
H1B1 H 0.1230(16) 0.0750(15) 0.7500 0.015(6) Uiso 1 2 d S . .
B2 B 0.57586(18) 0.16375(18) 0.7500 0.0221(6) Uani 1 2 d S . .
O1 O 0.47757(11) 0.10827(11) 0.7500 0.0259(4) Uani 1 2 d S . .
C7 C 0.44202(17) 0.01221(16) 0.7500 0.0321(6) Uani 1 2 d S . .
H7A H 0.4644 -0.0049 0.8090 0.039 Uiso 0.50 1 calc PR . .
H7B H 0.4644 -0.0049 0.6910 0.039 Uiso 0.50 1 calc PR . .
C8 C 0.34099(17) -0.03885(16) 0.7500 0.0299(6) Uani 1 2 d S . .
H8A H 0.3187 -0.0337 0.6851 0.036 Uiso 0.50 1 calc PR . .
H8B H 0.3185 -0.0135 0.8002 0.036 Uiso 0.50 1 calc PR . .
H8C H 0.3192 -0.1030 0.7647 0.036 Uiso 0.50 1 calc PR . .
O2 O 0.58531(10) 0.25552(10) 0.7500 0.0211(4) Uani 1 2 d S . .
B3 B 0.6667 0.3333 0.7500 0.0211(9) Uani 1 6 d S . .
O3 O 0.52700(8) 0.37674(8) 0.66701(10) 0.0252(3) Uani 1 1 d . . .
C9 C 0.56137(14) 0.40390(14) 0.57074(16) 0.0380(5) Uani 1 1 d . . .
H9A H 0.5978 0.3758 0.5506 0.046 Uiso 1 1 calc R A 1
H9B H 0.6001 0.4708 0.5668 0.046 Uiso 1 1 calc R A 1
C10 C 0.4790(7) 0.3713(7) 0.5064(9) 0.059(3) Uani 0.50 1 d P B 1
H10A H 0.4382 0.3061 0.5170 0.071 Uiso 0.50 1 calc PR B 1
H10B H 0.4978 0.3822 0.4371 0.071 Uiso 0.50 1 calc PR B 1
H10C H 0.4472 0.4044 0.5230 0.071 Uiso 0.50 1 calc PR B 1
C10' C 0.4965(8) 0.3479(8) 0.4926(9) 0.054(2) Uani 0.50 1 d P B 2
H10D H 0.4787 0.2839 0.5023 0.065 Uiso 0.50 1 calc PR B 2
H10E H 0.5254 0.3682 0.4279 0.065 Uiso 0.50 1 calc PR B 2
H10F H 0.4424 0.3544 0.4958 0.065 Uiso 0.50 1 calc PR B 2
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
O2 Ca1 O3 74.89(4) . 10_557
O2 Ca1 O3 74.89(4) . .
O3 Ca1 O3 55.19(6) 10_557 .
O2 Ca1 N3 155.90(6) . .
O3 Ca1 N3 83.80(5) 10_557 .
O3 Ca1 N3 83.80(5) . .
O2 Ca1 N1 121.51(4) . .
O3 Ca1 N1 153.64(5) 10_557 .
O3 Ca1 N1 106.24(5) . .
N3 Ca1 N1 74.97(5) . .
O2 Ca1 N1 121.51(4) . 10_557
O3 Ca1 N1 106.24(5) 10_557 10_557
O3 Ca1 N1 153.64(5) . 10_557
N3 Ca1 N1 74.97(5) . 10_557
N1 Ca1 N1 83.41(7) . 10_557
O2 Ca1 O1 54.24(5) . .
O3 Ca1 O1 122.35(4) 10_557 .
O3 Ca1 O1 122.35(4) . .
N3 Ca1 O1 149.85(6) . .
N1 Ca1 O1 82.68(4) . .
N1 Ca1 O1 82.68(4) 10_557 .
O2 Ca1 B2 62.88(6) . 3_665
O3 Ca1 B2 29.22(3) 10_557 3_665
O3 Ca1 B2 29.22(3) . 3_665
N3 Ca1 B2 93.02(7) . 3_665
N1 Ca1 B2 135.46(4) . 3_665
N1 Ca1 B2 135.46(4) 10_557 3_665
O1 Ca1 B2 117.13(6) . 3_665
O2 Ca1 B2 27.10(6) . .
O3 Ca1 B2 98.85(5) 10_557 .
O3 Ca1 B2 98.85(5) . .
N3 Ca1 B2 177.00(7) . .
N1 Ca1 B2 102.85(5) . .
N1 Ca1 B2 102.85(5) 10_557 .
O1 Ca1 B2 27.15(6) . .
B2 Ca1 B2 89.98(10) 3_665 .
C1 N1 N2 105.44(14) . .
C1 N1 Ca1 135.04(12) . .
N2 N1 Ca1 118.33(10) . .
C3 N2 N1 109.46(15) . .
C3 N2 B1 127.34(16) . .
N1 N2 B1 123.19(15) . .
N1 C1 C2 111.84(17) . .
C3 C2 C1 104.22(16) . .
N2 C3 C2 109.04(16) . .
C4 N3 N4 105.52(19) . .
C4 N3 Ca1 133.63(17) . .
N4 N3 Ca1 120.84(14) . .
C6 N4 N3 109.7(2) . .
C6 N4 B1 129.2(2) . .
N3 N4 B1 121.12(19) . .
N3 C4 C5 111.6(2) . .
C6 C5 C4 104.8(2) . .
N4 C6 C5 108.4(2) . .
N4 B1 N2 109.61(13) . 10_557
N4 B1 N2 109.61(13) . .
N2 B1 N2 111.0(2) 10_557 .
O1 B2 O3 116.22(13) . 11_657
O1 B2 O3 116.22(13) . 2_655
O3 B2 O3 100.24(18) 11_657 2_655
O1 B2 O2 99.63(18) . .
O3 B2 O2 112.59(14) 11_657 .
O3 B2 O2 112.59(14) 2_655 .
O1 B2 Ca1 157.03(16) . 2_655
O3 B2 Ca1 53.97(9) 11_657 2_655
O3 B2 Ca1 53.97(9) 2_655 2_655
O2 B2 Ca1 103.34(14) . 2_655
O1 B2 Ca1 52.96(11) . .
O3 B2 Ca1 129.57(9) 11_657 .
O3 B2 Ca1 129.57(9) 2_655 .
O2 B2 Ca1 46.67(10) . .
Ca1 B2 Ca1 150.02(9) 2_655 .
C7 O1 B2 115.73(18) . .
C7 O1 Ca1 144.38(14) . .
B2 O1 Ca1 99.90(13) . .
O1 C7 C8 111.8(2) . .
B3 O2 B2 123.17(15) . .
B3 O2 Ca1 130.60(9) . .
B2 O2 Ca1 106.23(13) . .
O2 B3 O2 120.0 2_655 .
O2 B3 O2 120.0 2_655 3_665
O2 B3 O2 120.0 . 3_665
C9 O3 B2 117.92(14) . 3_665
C9 O3 Ca1 135.27(11) . .
B2 O3 Ca1 96.81(10) 3_665 .
O3 C9 C10' 113.5(5) . .
O3 C9 C10 105.1(5) . .
C10' C9 C10 24.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O2 2.3719(16) .
Ca1 O3 2.4313(12) 10_557
Ca1 O3 2.4313(12) .
Ca1 N3 2.4580(19) .
Ca1 N1 2.4653(15) .
Ca1 N1 2.4653(15) 10_557
Ca1 O1 2.5365(16) .
Ca1 B2 2.985(3) 3_665
Ca1 B2 3.131(3) .
N1 C1 1.332(2) .
N1 N2 1.3667(19) .
N2 C3 1.350(2) .
N2 B1 1.544(2) .
C1 C2 1.386(3) .
C2 C3 1.365(3) .
N3 C4 1.319(3) .
N3 N4 1.366(3) .
N4 C6 1.346(3) .
N4 B1 1.537(3) .
C4 C5 1.383(4) .
C5 C6 1.361(4) .
B1 N2 1.544(2) 10_557
B2 O1 1.450(3) .
B2 O3 1.468(2) 11_657
B2 O3 1.468(2) 2_655
B2 O2 1.485(3) .
B2 Ca1 2.985(3) 2_655
O1 C7 1.429(3) .
C7 C8 1.486(4) .
O2 B3 1.3530(15) .
B3 O2 1.3530(15) 2_655
B3 O2 1.3530(15) 3_665
O3 C9 1.411(2) .
O3 B2 1.468(2) 3_665
C9 C10' 1.483(12) .
C9 C10 1.501(12) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 6.8 0.4
2 0.667 0.333 0.250 163.4 30.9
3 0.000 0.000 0.500 6.8 0.4
4 0.333 0.667 0.750 163.5 31.0
