#------------------------------------------------------------------------------ #$Date: 2008-02-29 13:03:34 +0200 (Fri, 29 Feb 2008) $ #$Revision: 179 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2015225.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_2015225 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 '[Mg (C9 H10 B N6)2], 2C H Cl3' _chemical_formula_moiety 'C18 H20 B2 Mg N12, 2C H Cl3' _chemical_formula_sum 'C20 H22 B2 Cl6 Mg N12' _chemical_formula_weight 689.13 _chemical_name_systematic ; bis[hydrotris(pyrazolyl)borato]magnesium(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 14.3475(12) _cell_length_b 14.3475(12) _cell_length_c 14.3475(12) _cell_measurement_reflns_used 600 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 20 _cell_volume 2953.4(4) _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 15868 _diffrn_reflns_theta_full 25.99 _diffrn_reflns_theta_max 25.99 _diffrn_reflns_theta_min 2.46 _diffrn_standards_decay_% 5 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_T_max 0.9447 _exptl_absorpt_correction_T_min 0.8827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1400 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.39 _refine_diff_density_min -0.36 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 63 _refine_ls_number_reflns 969 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.222 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0597 _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^)+(0.0339P)^2^+10.6109P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1229 _refine_ls_wR_factor_ref 0.1236 _reflns_number_gt 944 _reflns_number_total 969 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bm1623.cif 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_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' Mg Mg 0.0486 0.0363 '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' 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 Mg Mg 0.50000 0.50000 0.50000 0.0091(3) Uani 1.000 N N1 0.49046(18) 0.49637(19) 0.34889(19) 0.0120(8) Uani 1.000 N N2 0.43289(18) 0.43260(18) 0.30933(18) 0.0091(7) Uani 1.000 C C3 0.4397(2) 0.4362(2) 0.2163(2) 0.0137(9) Uani 1.000 C C4 0.5035(2) 0.5043(3) 0.1935(2) 0.0163(10) Uani 1.000 C C5 0.5332(2) 0.5398(2) 0.2789(2) 0.0151(9) Uani 1.000 B B1 0.3696(2) 0.3696(2) 0.3696(2) 0.0113(7) Uani 1.000 Cl Cl1 0.28234(6) 0.22160(6) 0.11889(6) 0.0224(3) Uani 1.000 C C6 0.1855(3) 0.1855(3) 0.1855(3) 0.0170(7) Uani 1.000 H H1 0.33018 0.33018 0.33018 0.0135 Uiso 1.000 H H3 0.40693 0.39921 0.17437 0.0164 Uiso 1.000 H H4 0.52249 0.52243 0.13423 0.0195 Uiso 1.000 H H5 0.57681 0.58726 0.28595 0.0181 Uiso 1.000 H H6 0.14604 0.14604 0.14604 0.0204 Uiso 1.000 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 Mg 0.0091(5) 0.0091(5) 0.0091(5) -0.0005(6) -0.0005(6) -0.0005(6) N1 0.0093(13) 0.0129(13) 0.0138(13) -0.0009(10) -0.0010(11) -0.0009(11) N2 0.0099(13) 0.0085(12) 0.0090(13) 0.0003(10) -0.0018(10) -0.0020(10) C3 0.0162(16) 0.0154(16) 0.0094(15) 0.0020(13) -0.0007(13) -0.0020(12) C4 0.0187(17) 0.0183(17) 0.0118(16) -0.0010(14) 0.0026(13) 0.0031(13) C5 0.0118(16) 0.0136(16) 0.0198(17) -0.0022(13) 0.0013(13) 0.0017(13) B1 0.0113(12) 0.0113(12) 0.0113(12) -0.0039(13) -0.0039(13) -0.0039(13) Cl1 0.0248(5) 0.0210(5) 0.0213(5) 0.0009(3) 0.0087(3) 0.0009(3) C6 0.0170(12) 0.0170(12) 0.0170(12) 0.0001(14) 0.0001(14) 0.0001(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Mg N1 2.173(3) yes N1 C5 1.331(4) no N1 N2 1.357(4) no N2 C3 1.339(4) no N2 B1 1.546(4) no C3 C4 1.378(5) no C4 C5 1.394(4) 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 1.764(4) 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 Cl1 N2 3.459(3) 23_554 no Cl1 N2 3.494(3) 20_554 no Cl1 C3 3.623(3) 20_554 no Cl1 C3 3.504(3) 23_554 no Cl1 H5 3.0900 6_564 no Cl1 H5 3.1100 4_645 no N1 N1 3.206(4) 21_666 no N1 N1 2.934(4) 5_555 no N1 N2 3.004(4) 5_555 no N1 N1 2.934(4) 9_555 no N1 N2 3.057(4) 9_555 no N1 N1 3.206(4) 17_666 no N2 N1 3.004(4) 9_555 no N2 Cl1 3.459(3) 18_555 no N2 N1 3.057(4) 5_555 no N2 Cl1 3.494(3) 22_555 no C3 Cl1 3.623(3) 22_555 no C3 Cl1 3.504(3) 18_555 no C3 H4 3.0400 6_564 no C4 H6 3.0300 15_555 no C4 H6 3.0300 19_555 no C4 H6 3.0300 22_555 no H3 H4 2.5200 6_564 no H4 C3 3.0400 11_655 no H4 H3 2.5200 11_655 no H5 Cl1 3.0900 11_655 no H5 Cl1 3.1100 4_655 no H6 C4 3.0300 15_545 no H6 C4 3.0300 20_554 no H6 C4 3.0300 24_455 no 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 Mg N1 5_555 84.94(10) yes Mg N1 N2 . 118.15(19) yes Mg N1 C5 . 135.4(2) yes N2 N1 C5 . 106.3(2) no N1 N2 C3 . 110.3(2) no N1 N2 B1 . 121.2(2) no C3 N2 B1 . 128.5(2) no N2 C3 C4 . 108.2(3) no C3 C4 C5 . 104.7(3) no N1 C5 C4 . 110.6(3) 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 . 125.00 no N1 C5 H5 . 125.00 no N2 B1 N2 9_555 108.2(2) no N2 B1 H1 . 111.00 no Cl1 C6 Cl1 5_555 110.8(2) no Cl1 C6 H6 . 108.00 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 Mg N1 N2 5_555 . -45.3(2) no N1 Mg N1 N2 9_555 . 40.1(2) no N1 Mg N1 N2 17_666 . 134.7(2) no N1 Mg N1 N2 21_666 . -139.9(2) no N1 Mg N1 C5 5_555 . 139.8(3) no N1 Mg N1 C5 9_555 . -134.9(3) no N1 Mg N1 C5 17_666 . -40.2(3) no N1 Mg N1 C5 21_666 . 45.1(3) no Mg N1 N2 C3 . . -176.28(19) no Mg N1 N2 B1 . . 5.0(3) no C5 N1 N2 C3 . . 0.0(3) no C5 N1 N2 B1 . . -178.7(2) no Mg N1 C5 C4 . . 175.4(2) no N2 N1 C5 C4 . . 0.0(4) no N1 N2 C3 C4 . . -0.1(3) no N1 N2 B1 N2 . 5_555 55.4(3) no B1 N2 C3 C4 . . 178.6(3) no C3 N2 B1 N2 . 9_555 119.9(3) no C3 N2 B1 N2 . 5_555 -123.2(3) no N1 N2 B1 N2 . 9_555 -61.6(3) no N2 C3 C4 C5 . . 0.0(4) no C3 C4 C5 N1 . . 0.0(4) no