#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:40:30 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301839 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/86/4338625.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_4338625
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            'C36 H40 B4 Ba2 N24'
_chemical_formula_weight         1126.84
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 119.481(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8850(11)
_cell_length_b                   15.9199(11)
_cell_length_c                   16.6548(13)
_cell_measurement_reflns_used    9446
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.9
_cell_measurement_theta_min      2.35
_cell_volume                     4589.7(6)
_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 0.922
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            87104
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         35.24
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.764
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.7084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick, 1997'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         9494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0267P)²+4.9850P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                8081
_reflns_number_total             9494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900342j_si_001.cif
_cod_data_source_block           lasy(2)
_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        4589.7(5)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4338625
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Ba1 Ba -0.145125(4) 0.502620(4) 0.417866(5) 0.01513(3) Uani 1 1 d . . .
N1 N -0.26332(7) 0.42070(8) 0.43578(9) 0.0245(2) Uani 1 1 d . A .
N2 N -0.33986(7) 0.43766(10) 0.37970(9) 0.0324(3) Uani 1 1 d . . .
C1 C -0.26046(10) 0.36405(10) 0.49649(11) 0.0290(3) Uani 1 1 d . . .
H1 H -0.2141 0.3401 0.5440 0.035 Uiso 1 1 calc R A .
C2 C -0.33426(11) 0.34445(12) 0.48131(13) 0.0386(4) Uani 1 1 d . A .
H2 H -0.3477 0.3066 0.5152 0.046 Uiso 1 1 calc R . .
C3 C -0.38246(10) 0.39171(13) 0.40701(13) 0.0401(5) Uani 1 1 d . A .
H3 H -0.4372 0.3924 0.3788 0.048 Uiso 1 1 calc R . .
N3 N -0.27224(8) 0.46702(11) 0.24650(10) 0.0327(3) Uani 1 1 d . A .
N4 N -0.34636(8) 0.47704(12) 0.22737(9) 0.0361(3) Uani 1 1 d . . .
C4 C -0.27653(12) 0.44922(13) 0.16570(12) 0.0401(4) Uani 1 1 d . . .
H4 H -0.2329 0.4394 0.1581 0.048 Uiso 1 1 calc R A .
C5 C -0.35200(13) 0.44687(14) 0.09454(12) 0.0462(5) Uani 1 1 d . A .
H5 H -0.3701 0.4352 0.0312 0.055 Uiso 1 1 calc R . .
C6 C -0.39452(11) 0.46521(16) 0.13600(12) 0.0456(5) Uani 1 1 d . A .
H6 H -0.4493 0.4691 0.1057 0.055 Uiso 1 1 calc R . .
N5 N -0.27529(19) 0.61045(19) 0.3728(2) 0.0209(6) Uiso 0.50 1 d P A 1
N6 N -0.34913(15) 0.57840(18) 0.33321(17) 0.0194(5) Uiso 0.50 1 d P A 1
C7 C -0.2812(2) 0.6905(2) 0.3933(2) 0.0290(6) Uiso 0.50 1 d P A 1
H7 H -0.2391 0.7285 0.4217 0.035 Uiso 0.50 1 calc PR A 1
C8 C -0.3572(2) 0.7106(3) 0.3673(3) 0.0337(7) Uiso 0.50 1 d P A 1
H8 H -0.3764 0.7632 0.3742 0.040 Uiso 0.50 1 calc PR A 1
C9 C -0.3985(2) 0.6387(2) 0.3299(2) 0.0292(6) Uiso 0.50 1 d P A 1
H9 H -0.4526 0.6322 0.3057 0.035 Uiso 0.50 1 calc PR A 1
B1 B -0.37042(19) 0.4872(2) 0.2989(2) 0.0186(6) Uiso 0.50 1 d P A 1
N5' N -0.2586(2) 0.6174(2) 0.3904(2) 0.0287(8) Uiso 0.50 1 d P A 2
N6' N -0.33539(17) 0.60155(19) 0.34353(19) 0.0231(5) Uiso 0.50 1 d P A 2
C7' C -0.2512(2) 0.6981(2) 0.4140(3) 0.0316(7) Uiso 0.50 1 d P A 2
H7' H -0.2035 0.7274 0.4451 0.038 Uiso 0.50 1 calc PR A 2
C8' C -0.3237(2) 0.7336(3) 0.3866(3) 0.0375(7) Uiso 0.50 1 d P A 2
H8' H -0.3344 0.7896 0.3967 0.045 Uiso 0.50 1 calc PR A 2
C9' C -0.3759(2) 0.6706(2) 0.3422(2) 0.0326(7) Uiso 0.50 1 d P A 2
H9' H -0.4304 0.6746 0.3154 0.039 Uiso 0.50 1 calc PR A 2
B1' B -0.3700(2) 0.5153(3) 0.3008(2) 0.0232(6) Uiso 0.50 1 d P A 2
B2 B -0.00739(9) 0.33652(9) 0.61579(10) 0.0180(2) Uani 1 1 d . . .
N7 N -0.09311(6) 0.33491(7) 0.44103(8) 0.0189(2) Uani 1 1 d . A .
N8 N -0.02552(7) 0.31083(7) 0.51663(8) 0.0183(2) Uani 1 1 d . A .
C10 C -0.10314(9) 0.28263(9) 0.37305(10) 0.0235(3) Uani 1 1 d . . .
H10 H -0.1455 0.2851 0.3120 0.028 Uiso 1 1 calc R A .
C11 C -0.04320(10) 0.22396(9) 0.40358(11) 0.0268(3) Uani 1 1 d . A .
H11 H -0.0368 0.1803 0.3690 0.032 Uiso 1 1 calc R . .
C12 C 0.00454(8) 0.24366(9) 0.49526(10) 0.0241(3) Uani 1 1 d . . .
H12 H 0.0507 0.2150 0.5365 0.029 Uiso 1 1 calc R A .
N9 N 0.00703(7) 0.49701(6) 0.60383(8) 0.01559(18) Uani 1 1 d . . .
N10 N -0.02818(6) 0.42978(7) 0.61907(7) 0.01592(18) Uani 1 1 d . A .
C13 C -0.02451(7) 0.56568(8) 0.61894(9) 0.0182(2) Uani 1 1 d . A .
H13 H -0.0107 0.6218 0.6138 0.022 Uiso 1 1 calc R . .
C14 C -0.08028(8) 0.54372(9) 0.64328(10) 0.0222(2) Uani 1 1 d . A .
H14 H -0.1113 0.5803 0.6566 0.027 Uiso 1 1 calc R . .
C15 C -0.08016(8) 0.45681(8) 0.64366(10) 0.0204(2) Uani 1 1 d . A .
H15 H -0.1112 0.4220 0.6586 0.024 Uiso 1 1 calc R . .
N11 N 0.07751(7) 0.31777(7) 0.68274(8) 0.0195(2) Uani 1 1 d . A .
N12 N 0.13761(7) 0.36442(8) 0.68939(9) 0.0257(2) Uani 1 1 d . . .
C16 C 0.10473(9) 0.25151(9) 0.74101(10) 0.0232(3) Uani 1 1 d . . .
H16 H 0.0740 0.2099 0.7485 0.028 Uiso 1 1 calc R A .
C17 C 0.18420(9) 0.25427(10) 0.78766(10) 0.0283(3) Uani 1 1 d . A .
H17 H 0.2191 0.2161 0.8328 0.034 Uiso 1 1 calc R . .
C18 C 0.20181(9) 0.32609(11) 0.75357(11) 0.0293(3) Uani 1 1 d . A .
H18 H 0.2528 0.3454 0.7733 0.035 Uiso 1 1 calc R . .
H1B1 H -0.4363(13) 0.5004(10) 0.2633(16) 0.025(6) Uiso 1 1 d . . .
H1B2 H -0.0449(10) 0.2979(10) 0.6341(11) 0.017(4) 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'
N N 0.0061 0.0033 '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'
Ba Ba -0.3244 2.2819 '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' Ba1 N3 73.10(8) . .
N5' Ba1 N7 149.77(8) . .
N3 Ba1 N7 91.97(4) . .
N5' Ba1 N12 72.06(8) . 5_566
N3 Ba1 N12 78.93(4) . 5_566
N7 Ba1 N12 131.83(4) . 5_566
N5' Ba1 N1 70.67(8) . .
N3 Ba1 N1 68.42(4) . .
N7 Ba1 N1 79.45(4) . .
N12 Ba1 N1 135.92(4) 5_566 .
N5' Ba1 N5 6.38(10) . .
N3 Ba1 N5 66.93(7) . .
N7 Ba1 N5 145.27(7) . .
N12 Ba1 N5 73.05(7) 5_566 .
N1 Ba1 N5 67.40(7) . .
N5' Ba1 N9 135.61(8) . 5_566
N3 Ba1 N9 107.81(4) . 5_566
N7 Ba1 N9 73.56(3) . 5_566
N12 Ba1 N9 64.97(3) 5_566 5_566
N1 Ba1 N9 152.66(3) . 5_566
N5 Ba1 N9 137.76(6) . 5_566
N5' Ba1 N9 120.19(8) . .
N3 Ba1 N9 165.78(4) . .
N7 Ba1 N9 73.92(3) . .
N12 Ba1 N9 109.02(3) 5_566 .
N1 Ba1 N9 109.62(3) . .
N5 Ba1 N9 126.17(7) . .
N9 Ba1 N9 67.04(4) 5_566 .
N5' Ba1 C13 95.57(8) . .
N3 Ba1 C13 168.34(4) . .
N7 Ba1 C13 96.85(3) . .
N12 Ba1 C13 100.53(4) 5_566 .
N1 Ba1 C13 105.68(3) . .
N5 Ba1 C13 101.66(7) . .
N9 Ba1 C13 82.10(3) 5_566 .
N9 Ba1 C13 24.75(3) . .
N5' Ba1 N10 121.67(8) . .
N3 Ba1 N10 145.27(4) . .
N7 Ba1 N10 59.13(3) . .
N12 Ba1 N10 134.03(3) 5_566 .
N1 Ba1 N10 86.33(3) . .
N5 Ba1 N10 125.71(6) . .
N9 Ba1 N10 83.60(3) 5_566 .
N9 Ba1 N10 25.01(3) . .
C13 Ba1 N10 39.64(3) . .
N5' Ba1 C14 83.68(8) . .
N3 Ba1 C14 146.68(4) . .
N7 Ba1 C14 96.75(3) . .
N12 Ba1 C14 116.62(4) 5_566 .
N1 Ba1 C14 81.64(3) . .
N5 Ba1 C14 88.68(7) . .
N9 Ba1 C14 105.50(3) 5_566 .
N9 Ba1 C14 40.66(3) . .
C13 Ba1 C14 24.41(3) . .
N10 Ba1 C14 39.30(3) . .
N5' Ba1 C15 99.20(8) . .
N3 Ba1 C15 138.51(4) . .
N7 Ba1 C15 74.42(3) . .
N12 Ba1 C15 138.74(4) 5_566 .
N1 Ba1 C15 70.59(3) . .
N5 Ba1 C15 102.70(6) . .
N9 Ba1 C15 105.48(3) 5_566 .
N9 Ba1 C15 39.91(3) . .
C13 Ba1 C15 38.94(3) . .
N10 Ba1 C15 23.44(3) . .
C14 Ba1 C15 23.55(4) . .
C1 N1 N2 105.64(13) . .
C1 N1 Ba1 131.55(11) . .
N2 N1 Ba1 122.76(9) . .
C3 N2 N1 109.51(15) . .
C3 N2 B1 124.99(19) . .
N1 N2 B1 125.06(17) . .
C3 N2 B1' 128.07(19) . .
N1 N2 B1' 121.83(16) . .
B1 N2 B1' 13.30(17) . .
N1 C1 C2 111.38(16) . .
C3 C2 C1 104.39(15) . .
N2 C3 C2 109.08(15) . .
C4 N3 N4 105.38(14) . .
C4 N3 Ba1 130.63(12) . .
N4 N3 Ba1 123.40(10) . .
C6 N4 N3 109.49(15) . .
C6 N4 B1 125.71(19) . .
N3 N4 B1 124.24(17) . .
C6 N4 B1' 126.2(2) . .
N3 N4 B1' 123.32(17) . .
B1 N4 B1' 15.79(16) . .
N3 C4 C5 111.95(17) . .
C6 C5 C4 104.06(15) . .
N4 C6 C5 109.12(17) . .
C7 N5 N6 105.5(3) . .
C7 N5 Ba1 132.9(3) . .
N6 N5 Ba1 120.9(2) . .
C9 N6 N5 109.7(3) . .
C9 N6 B1 126.2(3) . .
N5 N6 B1 124.0(2) . .
N5 C7 C8 111.0(3) . .
C9 C8 C7 105.5(3) . .
N6 C9 C8 108.3(3) . .
N2 B1 N4 122.9(3) . .
N2 B1 N6 105.2(2) . .
N4 B1 N6 105.0(2) . .
C7' N5' N6' 106.2(3) . .
C7' N5' Ba1 128.9(3) . .
N6' N5' Ba1 124.8(2) . .
N5' N6' C9' 110.5(3) . .
N5' N6' B1' 123.5(3) . .
C9' N6' B1' 126.0(3) . .
N5' C7' C8' 110.3(4) . .
C9' C8' C7' 105.4(3) . .
N6' C9' C8' 107.4(3) . .
N6' B1' N4 116.8(3) . .
N6' B1' N2 112.7(2) . .
N4 B1' N2 100.8(2) . .
N11 B2 N10 112.33(11) . .
N11 B2 N8 108.55(11) . .
N10 B2 N8 111.20(10) . .
C10 N7 N8 105.90(11) . .
C10 N7 Ba1 125.51(9) . .
N8 N7 Ba1 121.27(8) . .
C12 N8 N7 109.86(11) . .
C12 N8 B2 125.61(11) . .
N7 N8 B2 120.71(11) . .
N7 C10 C11 111.24(13) . .
C12 C11 C10 104.46(13) . .
N8 C12 C11 108.53(13) . .
C13 N9 N10 105.83(11) . .
C13 N9 Ba1 124.84(8) . 5_566
N10 N9 Ba1 128.17(7) . 5_566
C13 N9 Ba1 81.21(7) . .
N10 N9 Ba1 82.56(7) . .
Ba1 N9 Ba1 112.96(4) 5_566 .
C15 N10 N9 110.08(10) . .
C15 N10 B2 124.83(11) . .
N9 N10 B2 124.94(10) . .
C15 N10 Ba1 86.12(8) . .
N9 N10 Ba1 72.43(6) . .
B2 N10 Ba1 112.21(7) . .
N9 C13 C14 111.11(11) . .
N9 C13 Ba1 74.04(7) . .
C14 C13 Ba1 86.07(8) . .
C15 C14 C13 104.55(11) . .
C15 C14 Ba1 79.06(8) . .
C13 C14 Ba1 69.52(8) . .
N10 C15 C14 108.42(11) . .
N10 C15 Ba1 70.44(7) . .
C14 C15 Ba1 77.39(8) . .
C16 N11 N12 109.93(12) . .
C16 N11 B2 125.78(12) . .
N12 N11 B2 124.24(10) . .
C18 N12 N11 105.61(12) . .
C18 N12 Ba1 121.29(10) . 5_566
N11 N12 Ba1 132.39(8) . 5_566
N11 C16 C17 108.84(13) . .
C16 C17 C18 104.17(12) . .
N12 C18 C17 111.45(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ba1 N5' 2.760(4) .
Ba1 N3 2.7849(14) .
Ba1 N7 2.8204(12) .
Ba1 N12 2.8207(12) 5_566
Ba1 N1 2.8292(12) .
Ba1 N5 2.880(3) .
Ba1 N9 2.9407(11) 5_566
Ba1 N9 3.0873(12) .
Ba1 C13 3.1733(13) .
Ba1 N10 3.2112(11) .
Ba1 C14 3.3794(15) .
Ba1 C15 3.4001(14) .
N1 C1 1.3350(19) .
N1 N2 1.3648(18) .
N2 C3 1.356(2) .
N2 B1 1.413(4) .
N2 B1' 1.685(4) .
C1 C2 1.396(2) .
C2 C3 1.360(3) .
N3 C4 1.336(2) .
N3 N4 1.355(2) .
N4 C6 1.354(2) .
N4 B1 1.495(4) .
N4 B1' 1.629(4) .
C4 C5 1.381(3) .
C5 C6 1.361(3) .
N5 C7 1.340(5) .
N5 N6 1.378(4) .
N6 C9 1.355(4) .
N6 B1 1.542(5) .
C7 C8 1.388(5) .
C8 C9 1.368(5) .
N5' C7' 1.331(5) .
N5' N6' 1.354(5) .
N6' C9' 1.357(5) .
N6' B1' 1.543(5) .
C7' C8' 1.400(5) .
C8' C9' 1.369(5) .
B2 N11 1.5263(19) .
B2 N10 1.5493(18) .
B2 N8 1.5615(18) .
N7 C10 1.3387(18) .
N7 N8 1.3686(16) .
N8 C12 1.3554(18) .
C10 C11 1.398(2) .
C11 C12 1.380(2) .
N9 C13 1.3444(16) .
N9 N10 1.3694(14) .
N9 Ba1 2.9407(11) 5_566
N10 C15 1.3555(17) .
C13 C14 1.3997(18) .
C14 C15 1.384(2) .
N11 C16 1.3531(16) .
N11 N12 1.3645(16) .
N12 C18 1.3421(18) .
N12 Ba1 2.8207(12) 5_566
C16 C17 1.376(2) .
C17 C18 1.396(2) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139141225
