Synthesis, spectroscopic characterisation and X-ray structure of [trans-Co(en)~2~(NO~2~)~2~]~2~(Cr~2~O~7~)
Raj Pal Sharma; Rajni Sharma; Ritu Bala; Juan M. Salas; Miguel Quirós; Journal of Chemical Crystallography 35 (2005) 769–775; doi:10.1007/s10870-005-3886-9

data_1500012
_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 characterisation and
 X-ray structure of [trans-Co(en)~2~(NO~2~)~2~]~2~(Cr~2~O~7~)
;
_journal_issue                   10
_journal_name_full               'Journal of Chemical Crystallography'
_journal_page_first              769
_journal_page_last               775
_journal_paper_doi               10.1007/s10870-005-3886-9
_journal_volume                  35
_journal_year                    2005
_chemical_formula_sum            'C8 H32 Co2 Cr2 N12 O15'
_chemical_formula_weight         758.32
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.778(2)
_cell_length_b                   30.457(2)
_cell_length_c                   6.5364(5)
_cell_measurement_reflns_used    2692
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      2.68
_cell_volume                     4932.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Xtal_GX (S. Hall & D. du Boulay)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'phi and omega 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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7639
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_number         182
_exptl_absorpt_coefficient_mu    2.273
_exptl_absorpt_correction_T_max  0.8391
_exptl_absorpt_correction_T_min  0.6620
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    2.042
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2779
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0800P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                2556
_reflns_number_total             2779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            conitdcr.cif
_cod_data_source_block           conitdcr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorrombic' was replaced with
'orthorhombic' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               1500012