#------------------------------------------------------------------------------
#$Date: 2018-08-22 02:00:00 +0300 (Wed, 22 Aug 2018) $
#$Revision: 210037 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/33/86/4338626.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_4338626
loop_
_publ_author_name
'Saly, Mark J.'
'Heeg, Mary Jane'
'Winter, Charles H.'
_publ_section_title
;
 Volatility, High Thermal Stability, and Low Melting Points in Heavier
 Alkaline Earth Metal Complexes Containing Tris(pyrazolyl)borate Ligands
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5303
_journal_page_last               5312
_journal_paper_doi               10.1021/ic900342j
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C42 H68 B2 Ca N12'
_chemical_formula_weight         802.78
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 106.084(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.0949(4)
_cell_length_b                   12.5709(4)
_cell_length_c                   16.6206(6)
_cell_measurement_reflns_used    5168
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.6
_cell_measurement_theta_min      2.6
_cell_volume                     2227.38(14)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0830
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            65160
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.9551
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.426
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5566
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0767
_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)+(0.1176P)²+0.9711P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2024
_refine_ls_wR_factor_ref         0.2263
_reflns_number_gt                3733
_reflns_number_total             5566
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900342j_si_001.cif
_cod_data_source_block           catp(5)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2227.38(13)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4338626
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.5000 0.0000 0.0000 0.0282(2) Uani 1 2 d S . .
N1 N 0.7091(2) -0.01272(17) 0.10135(15) 0.0296(5) Uani 1 1 d . . .
N2 N 0.78721(19) 0.07376(17) 0.10966(14) 0.0272(5) Uani 1 1 d . . .
C1 C 0.7602(2) -0.0770(2) 0.16573(17) 0.0302(6) Uani 1 1 d . . .
C2 C 0.8709(3) -0.0326(2) 0.21573(18) 0.0333(6) Uani 1 1 d . . .
H2 H 0.9256 -0.0625 0.2649 0.040 Uiso 1 1 calc R . .
C3 C 0.8849(2) 0.0632(2) 0.17926(17) 0.0284(6) Uani 1 1 d . . .
C4 C 0.6991(3) -0.1801(2) 0.1774(2) 0.0386(7) Uani 1 1 d . . .
H4A H 0.6410 -0.2018 0.1232 0.046 Uiso 1 1 calc R . .
H4B H 0.6489 -0.1690 0.2175 0.046 Uiso 1 1 calc R . .
C5 C 0.7918(3) -0.2687(3) 0.2093(2) 0.0491(8) Uani 1 1 d . . .
H5A H 0.8386 -0.2831 0.1684 0.059 Uiso 1 1 calc R . .
H5B H 0.7466 -0.3331 0.2174 0.059 Uiso 1 1 calc R . .
H5C H 0.8502 -0.2476 0.2627 0.059 Uiso 1 1 calc R . .
C6 C 0.9866(3) 0.1452(2) 0.20699(19) 0.0368(7) Uani 1 1 d . . .
H6A H 0.9480 0.2168 0.1999 0.044 Uiso 1 1 calc R . .
H6B H 1.0433 0.1408 0.1704 0.044 Uiso 1 1 calc R . .
C7 C 1.0636(3) 0.1317(3) 0.2977(2) 0.0448(8) Uani 1 1 d . . .
H7A H 1.0082 0.1355 0.3343 0.054 Uiso 1 1 calc R . .
H7B H 1.1264 0.1885 0.3125 0.054 Uiso 1 1 calc R . .
H7C H 1.1059 0.0625 0.3045 0.054 Uiso 1 1 calc R . .
N3 N 0.5343(2) 0.1860(2) 0.04665(15) 0.0369(6) Uani 1 1 d . . .
N4 N 0.6481(2) 0.23228(18) 0.05104(15) 0.0336(5) Uani 1 1 d . . .
C8 C 0.4581(3) 0.2657(3) 0.05503(19) 0.0440(8) Uani 1 1 d . . .
C9 C 0.5227(3) 0.3627(3) 0.0650(2) 0.0474(8) Uani 1 1 d . . .
H9 H 0.4899 0.4309 0.0718 0.057 Uiso 1 1 calc R . .
C10 C 0.6427(3) 0.3396(3) 0.0630(2) 0.0443(8) Uani 1 1 d . . .
C11 C 0.3251(3) 0.2424(3) 0.0532(2) 0.0556(10) Uani 1 1 d . . .
H11A H 0.3133 0.1643 0.0532 0.067 Uiso 1 1 calc R . .
H11B H 0.2689 0.2706 0.0005 0.067 Uiso 1 1 calc R . .
C12 C 0.2875(4) 0.2894(3) 0.1259(3) 0.0675(12) Uani 1 1 d . . .
H12A H 0.3369 0.2564 0.1780 0.081 Uiso 1 1 calc R . .
H12B H 0.1981 0.2761 0.1188 0.081 Uiso 1 1 calc R . .
H12C H 0.3030 0.3662 0.1281 0.081 Uiso 1 1 calc R . .
C13 C 0.7517(4) 0.4138(3) 0.0733(3) 0.0654(11) Uani 1 1 d . . .
H13A H 0.7353 0.4776 0.1035 0.078 Uiso 1 1 calc R . .
H13B H 0.8269 0.3784 0.1098 0.078 Uiso 1 1 calc R . .
C14 C 0.7816(6) 0.4487(5) -0.0012(3) 0.0968(17) Uani 1 1 d . . .
H14A H 0.8042 0.3871 -0.0302 0.116 Uiso 1 1 calc R . .
H14B H 0.8524 0.4983 0.0139 0.116 Uiso 1 1 calc R . .
H14C H 0.7086 0.4844 -0.0382 0.116 Uiso 1 1 calc R . .
N5 N 0.6322(2) 0.06650(19) -0.08544(14) 0.0307(5) Uani 1 1 d . . .
N6 N 0.7400(2) 0.12110(18) -0.04508(14) 0.0301(5) Uani 1 1 d . . .
C15 C 0.6436(3) 0.0408(2) -0.16089(19) 0.0348(6) Uani 1 1 d . B .
C16 C 0.7584(3) 0.0770(3) -0.1694(2) 0.0435(8) Uani 1 1 d . . .
H16 H 0.7897 0.0688 -0.2168 0.052 Uiso 1 1 calc R . .
C17 C 0.8169(3) 0.1269(3) -0.0955(2) 0.0406(7) Uani 1 1 d . D .
C18 C 0.5419(3) -0.0198(3) -0.2229(2) 0.0428(8) Uani 1 1 d . . .
H18A H 0.4648 0.0241 -0.2372 0.051 Uiso 1 1 calc R A 1
H18B H 0.5236 -0.0853 -0.1954 0.051 Uiso 1 1 calc R A 1
C19 C 0.5715(7) -0.0513(6) -0.3046(5) 0.0400(16) Uani 0.50 1 d P B 1
H19A H 0.5971 0.0119 -0.3302 0.048 Uiso 0.50 1 calc PR B 1
H19B H 0.4966 -0.0824 -0.3433 0.048 Uiso 0.50 1 calc PR B 1
H19C H 0.6397 -0.1036 -0.2924 0.048 Uiso 0.50 1 calc PR B 1
C19' C 0.5461(11) 0.0172(10) -0.3105(6) 0.080(3) Uani 0.50 1 d P B 2
H19D H 0.5471 0.0951 -0.3123 0.096 Uiso 0.50 1 calc PR B 2
H19E H 0.4720 -0.0094 -0.3527 0.096 Uiso 0.50 1 calc PR B 2
H19F H 0.6220 -0.0106 -0.3223 0.096 Uiso 0.50 1 calc PR B 2
C20 C 0.9485(3) 0.1722(3) -0.0688(2) 0.0530(9) Uani 1 1 d . . .
H20A H 0.9744 0.1916 -0.1193 0.064 Uiso 1 1 calc R C 1
H20B H 0.9484 0.2379 -0.0359 0.064 Uiso 1 1 calc R C 1
C21 C 1.0371(5) 0.0990(6) -0.0198(5) 0.0502(18) Uani 0.50 1 d P D 1
H21A H 1.1204 0.1320 -0.0034 0.060 Uiso 0.50 1 calc PR D 1
H21B H 1.0395 0.0348 -0.0527 0.060 Uiso 0.50 1 calc PR D 1
H21C H 1.0122 0.0800 0.0306 0.060 Uiso 0.50 1 calc PR D 1
C21' C 0.9454(10) 0.2816(8) -0.0882(8) 0.094(3) Uani 0.50 1 d P D 2
H21D H 1.0300 0.3113 -0.0680 0.113 Uiso 0.50 1 calc PR D 2
H21E H 0.8892 0.3184 -0.0611 0.113 Uiso 0.50 1 calc PR D 2
H21F H 0.9147 0.2911 -0.1490 0.113 Uiso 0.50 1 calc PR D 2
B1 B 0.7622(3) 0.1649(3) 0.0443(2) 0.0304(7) Uani 1 1 d . . .
H1B1 H 0.850(3) 0.218(3) 0.055(2) 0.041(9) 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'
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
N5 Ca1 N5 180.00(14) . 3_655
N5 Ca1 N3 101.93(8) . 3_655
N5 Ca1 N3 78.07(8) 3_655 3_655
N5 Ca1 N3 78.07(8) . .
N5 Ca1 N3 101.93(8) 3_655 .
N3 Ca1 N3 180.00(12) 3_655 .
N5 Ca1 N1 79.49(7) . .
N5 Ca1 N1 100.51(7) 3_655 .
N3 Ca1 N1 100.83(7) 3_655 .
N3 Ca1 N1 79.17(7) . .
N5 Ca1 N1 100.51(7) . 3_655
N5 Ca1 N1 79.49(7) 3_655 3_655
N3 Ca1 N1 79.17(7) 3_655 3_655
N3 Ca1 N1 100.83(7) . 3_655
N1 Ca1 N1 180.00(17) . 3_655
C1 N1 N2 106.4(2) . .
C1 N1 Ca1 134.21(18) . .
N2 N1 Ca1 117.75(15) . .
C3 N2 N1 110.0(2) . .
C3 N2 B1 128.0(2) . .
N1 N2 B1 122.0(2) . .
N1 C1 C2 110.2(2) . .
N1 C1 C4 121.3(2) . .
C2 C1 C4 128.5(3) . .
C3 C2 C1 106.0(2) . .
N2 C3 C2 107.5(2) . .
N2 C3 C6 123.3(2) . .
C2 C3 C6 129.2(3) . .
C1 C4 C5 113.3(2) . .
C3 C6 C7 113.3(3) . .
C8 N3 N4 105.9(3) . .
C8 N3 Ca1 134.0(2) . .
N4 N3 Ca1 118.64(16) . .
C10 N4 N3 110.4(2) . .
C10 N4 B1 128.1(3) . .
N3 N4 B1 121.4(2) . .
N3 C8 C9 110.2(3) . .
N3 C8 C11 119.9(3) . .
C9 C8 C11 129.9(3) . .
C10 C9 C8 106.3(3) . .
N4 C10 C9 107.1(3) . .
N4 C10 C13 124.3(3) . .
C9 C10 C13 128.5(3) . .
C8 C11 C12 113.5(3) . .
C14 C13 C10 117.5(4) . .
C15 N5 N6 106.4(2) . .
C15 N5 Ca1 133.54(19) . .
N6 N5 Ca1 117.67(16) . .
C17 N6 N5 109.6(2) . .
C17 N6 B1 128.2(2) . .
N5 N6 B1 122.2(2) . .
N5 C15 C16 110.1(3) . .
N5 C15 C18 121.2(3) . .
C16 C15 C18 128.8(3) . .
C17 C16 C15 106.1(3) . .
N6 C17 C16 107.8(3) . .
N6 C17 C20 124.1(3) . .
C16 C17 C20 127.8(3) . .
C15 C18 C19 115.6(4) . .
C15 C18 C19' 106.3(4) . .
C19 C18 C19' 34.2(5) . .
C21' C20 C21 136.8(6) . .
C21' C20 C17 109.8(5) . .
C21 C20 C17 112.4(4) . .
N6 B1 N2 111.2(2) . .
N6 B1 N4 110.4(2) . .
N2 B1 N4 110.1(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 N5 2.453(2) .
Ca1 N5 2.453(2) 3_655
Ca1 N3 2.460(2) 3_655
Ca1 N3 2.460(2) .
Ca1 N1 2.465(2) .
Ca1 N1 2.465(2) 3_655
N1 C1 1.335(3) .
N1 N2 1.373(3) .
N2 C3 1.355(3) .
N2 B1 1.550(4) .
C1 C2 1.394(4) .
C1 C4 1.501(4) .
C2 C3 1.377(4) .
C3 C6 1.503(4) .
C4 C5 1.508(4) .
C6 C7 1.522(4) .
N3 C8 1.343(4) .
N3 N4 1.373(3) .
N4 C10 1.367(4) .
N4 B1 1.553(4) .
C8 C9 1.400(5) .
C8 C11 1.497(5) .
C9 C10 1.372(5) .
C10 C13 1.499(5) .
C11 C12 1.503(5) .
C13 C14 1.437(7) .
N5 C15 1.335(4) .
N5 N6 1.381(3) .
N6 C17 1.354(4) .
N6 B1 1.540(4) .
C15 C16 1.397(4) .
C15 C18 1.507(4) .
C16 C17 1.372(5) .
C17 C20 1.514(4) .
C18 C19 1.534(7) .
C18 C19' 1.541(11) .
C20 C21' 1.410(11) .
C20 C21 1.426(8) .
