#------------------------------------------------------------------------------ #$Date: 2014-07-11 17:35:18 +0300 (Fri, 11 Jul 2014) $ #$Revision: 120071 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/50/00/1500010.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_1500010 loop_ _publ_author_name 'Raj Pal Sharma' 'Bal Krishan Vermani' 'Rajni Sharma' 'Ritu Bala' 'Dip Singh Gill' 'Juan M. Salas' 'Miguel Quir\'os' _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica Facultad de Ciencias Universidad de Granada 18071 Granada SPAIN ; _publ_contact_author_email mquiros@ugr.es _publ_contact_author_fax 34-58-248526 _publ_contact_author_name 'Miguel Quir\'os' _publ_contact_author_phone 34-58-240441 _publ_section_title ; Synthesis, spectroscopic characterization and X-ray structure determinations and packing of tetralkylammonium trans-diamminetetranitrocobaltate(III) complex salts where alkyl = methyl or ehtyl ; _journal_name_full 'Journal of Molecular Structure' _journal_page_first 222 _journal_page_last 227 _journal_volume 784 _journal_year 2006 _chemical_formula_sum 'C4 H18 Co N7 O8' _chemical_formula_weight 351.18 _chemical_name_systematic ; ? ; _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 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 90.078(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.1926(7) _cell_length_b 18.248(3) _cell_length_c 6.2335(6) _cell_measurement_reflns_used 35 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 12.43 _cell_measurement_theta_min 4.64 _cell_volume 704.41(16) _computing_cell_refinement 'Siemens XSCANS' _computing_data_collection 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _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 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 3406 _diffrn_reflns_theta_full 32.50 _diffrn_reflns_theta_max 32.50 _diffrn_reflns_theta_min 2.23 _diffrn_standards_decay_% 7.92 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.268 _exptl_absorpt_correction_T_max 0.7786 _exptl_absorpt_correction_T_min 0.6546 _exptl_absorpt_correction_type psi-scan _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular shape' _exptl_crystal_F_000 364 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.425 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.181 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.236 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 107 _refine_ls_number_reflns 2630 _refine_ls_number_restraints 10 _refine_ls_restrained_S_all 1.234 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0868 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2891 _refine_ls_wR_factor_ref 0.2981 _reflns_number_gt 2110 _reflns_number_total 2630 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file coinmet.cif _[local]_cod_data_source_block coinmet _[local]_cod_cif_authors_sg_H-M 'P 2(1)/m ' _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced with 'psi-scan' value. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_database_code 1500010 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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 Co Co 0.5000 0.5000 0.5000 0.0239(3) Uani 1 2 d S N1M N 0.3247(8) 0.5269(3) 0.2521(8) 0.0380(10) Uani 1 1 d . H1M H 0.3252 0.4904 0.1573 0.046 Uiso 1 1 d R H2M H 0.3791 0.5670 0.1916 0.046 Uiso 1 1 d R H3M H 0.1897 0.5356 0.2940 0.046 Uiso 1 1 d R N1N N 0.2443(8) 0.4565(3) 0.6309(8) 0.0378(10) Uani 1 1 d . O1N O 0.1115(8) 0.4240(3) 0.5135(8) 0.0512(12) Uani 1 1 d . O2N O 0.2155(10) 0.4596(4) 0.8232(8) 0.0667(17) Uani 1 1 d . N2N N 0.5596(8) 0.4036(3) 0.3727(9) 0.0403(10) Uani 1 1 d . O3N O 0.6049(11) 0.3518(3) 0.4923(9) 0.0582(14) Uani 1 1 d . O4N O 0.5441(11) 0.3950(3) 0.1781(8) 0.0622(15) Uani 1 1 d . N1C N 0.0680(13) 0.2500 -0.0032(12) 0.0399(14) Uani 1 2 d SD C1C C 0.040(3) 0.3136(7) 0.128(3) 0.136(7) Uani 1 1 d . H11C H 0.0693 0.3568 0.0438 0.163 Uiso 1 1 d R H12C H 0.1395 0.3121 0.2476 0.163 Uiso 1 1 d R H13C H -0.1052 0.3161 0.1822 0.163 Uiso 1 1 d R C2C C 0.269(3) 0.2500 -0.128(4) 0.119(8) Uani 1 2 d SD H21C H 0.354(3) 0.2927 -0.097(6) 0.143 Uiso 1 1 d D H22C H 0.238(7) 0.2500 -0.279(3) 0.143 Uiso 1 2 d SD C3C C -0.101(4) 0.2500 -0.165(4) 0.171(15) Uani 1 2 d SD H31C H -0.192(4) 0.2927 -0.150(6) 0.205 Uiso 1 1 d D H32C H -0.043(7) 0.2500 -0.308(3) 0.205 Uiso 1 2 d SD loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0237(4) 0.0282(4) 0.0198(4) 0.0006(3) 0.0003(3) -0.0005(3) N1M 0.036(2) 0.047(3) 0.031(2) 0.0040(19) -0.0019(17) 0.000(2) N1N 0.032(2) 0.048(3) 0.033(2) 0.0009(19) 0.0013(16) -0.0042(19) O1N 0.039(2) 0.063(3) 0.052(3) -0.007(2) 0.0024(19) -0.018(2) O2N 0.057(3) 0.107(5) 0.036(2) 0.005(3) 0.009(2) -0.019(3) N2N 0.037(2) 0.039(2) 0.044(3) -0.003(2) 0.0031(19) 0.0015(19) O3N 0.083(4) 0.036(2) 0.055(3) 0.004(2) 0.001(3) 0.009(2) O4N 0.087(4) 0.062(3) 0.038(2) -0.016(2) 0.004(2) 0.008(3) N1C 0.038(3) 0.036(3) 0.046(4) 0.000 0.002(3) 0.000 C1C 0.192(19) 0.069(7) 0.146(14) -0.038(8) 0.074(13) -0.013(9) C2C 0.075(11) 0.150(19) 0.133(17) 0.000 0.058(12) 0.000 C3C 0.098(17) 0.31(5) 0.105(17) 0.000 -0.027(14) 0.000 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' 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' Co Co 0.3494 0.9721 '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 N1M Co N1M 180.0(2) . 3_666 N1M Co N1N 89.0(2) . . N1M Co N1N 91.0(2) 3_666 . N1M Co N1N 91.0(2) . 3_666 N1M Co N1N 89.0(2) 3_666 3_666 N1N Co N1N 179.999(2) . 3_666 N1M Co N2N 90.6(2) . . N1M Co N2N 89.4(2) 3_666 . N1N Co N2N 87.6(2) . . N1N Co N2N 92.4(2) 3_666 . N1M Co N2N 89.4(2) . 3_666 N1M Co N2N 90.6(2) 3_666 3_666 N1N Co N2N 92.4(2) . 3_666 N1N Co N2N 87.6(2) 3_666 3_666 N2N Co N2N 180.0(3) . 3_666 O2N N1N O1N 120.2(5) . . O2N N1N Co 121.0(4) . . O1N N1N Co 118.8(4) . . O4N N2N O3N 121.0(6) . . O4N N2N Co 120.0(5) . . O3N N2N Co 118.9(4) . . C1C N1C C1C 108.5(14) . 4_565 C1C N1C C3C 108.1(11) . . C1C N1C C3C 108.1(11) 4_565 . C1C N1C C2C 113.8(9) . . C1C N1C C2C 113.8(9) 4_565 . C3C N1C C2C 104.1(14) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Co N1M 1.950(5) . Co N1M 1.950(5) 3_666 Co N1N 1.951(5) . Co N1N 1.951(5) 3_666 Co N2N 1.965(5) . Co N2N 1.965(5) 3_666 N1N O2N 1.214(7) . N1N O1N 1.249(7) . N2N O4N 1.227(7) . N2N O3N 1.236(7) . N1C C1C 1.430(13) . N1C C1C 1.430(13) 4_565 N1C C3C 1.453(19) . N1C C2C 1.470(15) . _journal_paper_doi 10.1016/j.molstruc.2005.09.008