Synthesis, spectroscopic characterization and X-ray structure determinations and packing of tetralkylammonium trans-diamminetetranitrocobaltate(III) complex salts where alkyl = methyl or ehtyl
Raj Pal Sharma; Bal Krishan Vermani; Rajni Sharma; Ritu Bala; Dip Singh Gill; Juan M. Salas; Miguel Quirós; Journal of Molecular Structure 784 (2006) 222–227; doi:10.1016/j.molstruc.2005.09.008

data_1500010
_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_paper_doi               10.1016/j.molstruc.2005.09.008
_journal_volume                  784
_journal_year                    2006
_chemical_formula_sum            'C4 H18 Co N7 O8'
_chemical_formula_weight         351.18
_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)
_cod_data_source_file            coinmet.cif
_cod_data_source_block           coinmet
_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_original_sg_symbol_H-M      'P 2(1)/m  '
_cod_database_code               1500010