#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/52/2015226.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2015226 loop_ _publ_author_name 'Mar\'ia Gabriela-Ballinas-L\'opez' 'Itzia I. Padilla-Mart\'inez' 'Francisco J. Mart\'inez-Mart\'inez' 'Herbert H\"opfl' 'Efr\'en V. Garc\'ia-B\'aez' _publ_section_title ; Facial \p...Cl...\p interactions as the directing motif of the supramolecular structure of bis-hydrotris(pyrazolyl)borates of Mg^2+^ and Ca^2+^ chloroform disolvates ; _journal_coeditor_code BM1623 _journal_issue 4 _journal_name_full 'Acta Crystallographica, Section C' _journal_page_first m132 _journal_page_last m135 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Ca (C9 H10 B N6)2], 2C H Cl3' _chemical_formula_moiety 'C18 H20 B2 Ca N12, 2C H Cl3' _chemical_formula_sum 'C20 H22 B2 Ca Cl6 N12' _chemical_formula_weight 704.90 _chemical_name_systematic ; bis[hydrotris(pyrazolyl)borato]calcium(II) chloroform disolvate ; _symmetry_cell_setting cubic _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P a -3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 14.6697(9) _cell_length_b 14.6697(9) _cell_length_c 14.6697(9) _cell_measurement_reflns_used 600 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 20 _cell_volume 3156.9(3) _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction SAINT _computing_molecular_graphics 'Mercury 1.4 (Bruno et al., 2002)' _computing_publication_material 'SHELXL97 and WINGX-2003 (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 17681 _diffrn_reflns_theta_full 28.26 _diffrn_reflns_theta_max 28.26 _diffrn_reflns_theta_min 2.40 _diffrn_standards_decay_% 5 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_T_max 0.8659 _exptl_absorpt_correction_T_min 0.8082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1432 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.44 _refine_diff_density_min -0.40 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.308 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 63 _refine_ls_number_reflns 1293 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.308 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0514 _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/[\s^2^(Fo^2^)+(0.0316P)^2^+4.1829P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1082 _refine_ls_wR_factor_ref 0.1085 _reflns_number_gt 1272 _reflns_number_total 1293 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bm1623.cif _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2015226 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z 5 z,x,y 6 1/2-z,-x,1/2+y 7 1/2+z,1/2-x,-y 8 -z,1/2+x,1/2-y 9 y,z,x 10 1/2+y,1/2-z,-x 11 -y,1/2+z,1/2-x 12 1/2-y,-z,1/2+x 13 -x,-y,-z 14 1/2+x,y,1/2-z 15 1/2-x,1/2+y,z 16 x,1/2-y,1/2+z 17 -z,-x,-y 18 1/2+z,x,1/2-y 19 1/2-z,1/2+x,y 20 z,1/2-x,1/2+y 21 -y,-z,-x 22 1/2-y,1/2+z,x 23 y,1/2-z,1/2+x 24 1/2+y,z,1/2-x loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ca 0.0141(2) 0.0141(2) 0.0141(2) -0.0023(2) -0.0023(2) -0.0023(2) N1 0.0184(9) 0.0214(9) 0.0177(9) -0.0059(7) -0.0014(7) 0.0005(7) N2 0.0151(8) 0.0167(8) 0.0125(8) -0.0001(6) -0.0001(6) -0.0002(6) C3 0.0241(11) 0.0239(10) 0.0141(9) -0.0014(9) -0.0011(8) -0.0022(8) C4 0.0287(12) 0.0282(12) 0.0167(10) -0.0036(9) 0.0038(9) 0.0027(9) C5 0.0215(10) 0.0255(11) 0.0205(10) -0.0057(9) 0.0022(8) 0.0030(8) B1 0.0146(7) 0.0146(7) 0.0146(7) -0.0013(8) -0.0013(8) -0.0013(8) Cl1 0.0416(4) 0.0370(4) 0.0341(3) -0.0098(3) 0.0157(3) -0.0097(3) C6 0.0237(8) 0.0237(8) 0.0237(8) -0.0017(9) -0.0017(9) -0.0017(9) loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy Ca Ca 0.50000 0.50000 0.50000 0.01410(10) Uani 1.000 N N1 0.48740(12) 0.48337(13) 0.33608(12) 0.0192(5) Uani 1.000 N N2 0.42579(11) 0.42280(11) 0.30197(11) 0.0148(5) Uani 1.000 C C3 0.42747(16) 0.42495(15) 0.21011(14) 0.0207(6) Uani 1.000 C C4 0.49139(16) 0.48835(16) 0.18296(15) 0.0245(7) Uani 1.000 C C5 0.52681(15) 0.52263(16) 0.26431(15) 0.0225(6) Uani 1.000 B B1 0.36350(15) 0.36350(15) 0.36350(15) 0.0146(4) Uani 1.000 Cl Cl1 0.28142(5) 0.21172(5) 0.12085(5) 0.0376(2) Uani 1.000 C C6 0.18308(16) 0.18308(16) 0.18308(16) 0.0237(5) Uani 1.000 H H1 0.32493 0.32493 0.32493 0.0175 Uiso 1.000 H H3 0.39159 0.38966 0.17156 0.0248 Uiso 1.000 H H4 0.50730 0.50458 0.12378 0.0294 Uiso 1.000 H H5 0.57195 0.56700 0.26794 0.0270 Uiso 1.000 H H6 0.14451 0.14451 0.14451 0.0284 Uiso 1.000 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' Cl Cl 0.1484 0.1585 '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_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Ca N1 5_555 79.45(6) yes Ca N1 N2 . 118.72(12) yes Ca N1 C5 . 135.03(15) yes N2 N1 C5 . 106.23(17) no N1 N2 C3 . 109.86(17) no N1 N2 B1 . 122.87(16) no C3 N2 B1 . 127.26(17) no N2 C3 C4 . 108.47(19) no C3 C4 C5 . 104.43(19) no N1 C5 C4 . 111.0(2) no N2 C3 H3 . 126.00 no C4 C3 H3 . 126.00 no C3 C4 H4 . 128.00 no C5 C4 H4 . 128.00 no C4 C5 H5 . 124.00 no N1 C5 H5 . 124.00 no N2 B1 N2 9_555 109.80(16) no N2 B1 H1 . 109.00 no Cl1 C6 Cl1 5_555 110.74(13) no Cl1 C6 H6 . 108.00 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ca N1 2.4241(18) yes N1 C5 1.332(3) no N1 N2 1.363(2) no N2 C3 1.348(3) no N2 B1 1.551(3) no C3 C4 1.380(3) no C4 C5 1.395(3) no C3 H3 0.9300 no C4 H4 0.9300 no C5 H5 0.9300 no C6 H6 0.9800 no B1 H1 0.9800 no Cl1 C6 1.758(2) no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag N1 N1 3.098(3) 5_555 no N1 N2 3.120(2) 5_555 no N1 N1 3.098(3) 9_555 no N1 N2 3.116(2) 9_555 no N2 N1 3.116(2) 5_555 no N2 N1 3.120(2) 9_555 no C4 H6 3.0900 15_555 no C4 H6 3.0900 19_555 no C4 H6 3.0900 22_555 no C4 H4 3.0600 23_554 no H4 C4 3.0600 18_555 no H4 H4 2.5400 18_555 no H4 H4 2.5400 23_554 no H6 C4 3.0900 15_545 no H6 C4 3.0900 20_554 no H6 C4 3.0900 24_455 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 Ca N1 N2 5_555 . -40.39(14) no N1 Ca N1 N2 9_555 . 40.70(14) no N1 Ca N1 N2 17_666 . 139.61(14) no N1 Ca N1 N2 21_666 . -139.30(14) no N1 Ca N1 C5 5_555 . 137.7(2) no N1 Ca N1 C5 9_555 . -141.3(2) no N1 Ca N1 C5 17_666 . -42.4(2) no N1 Ca N1 C5 21_666 . 38.8(2) no Ca N1 N2 C3 . . 178.57(14) no Ca N1 N2 B1 . . -0.3(2) no C5 N1 N2 C3 . . 0.0(2) no C5 N1 N2 B1 . . -178.87(18) no Ca N1 C5 C4 . . -178.12(16) no N2 N1 C5 C4 . . 0.1(2) no N1 N2 C3 C4 . . -0.1(2) no N1 N2 B1 N2 . 5_555 60.6(2) no B1 N2 C3 C4 . . 178.71(19) no C3 N2 B1 N2 . 9_555 121.1(2) no C3 N2 B1 N2 . 5_555 -118.1(2) no N1 N2 B1 N2 . 9_555 -60.2(2) no N2 C3 C4 C5 . . 0.2(3) no C3 C4 C5 N1 . . -0.2(3) no