Bis[tris(ethane-1,2-diamine)nickel(II)] octacyanidomolybdate(IV) dihydrate
Liu, Wen-Yan; Zhou, Hu; Guo, Ji-Xi; Yuan, Ai-Hua; Acta Crystallographica Section E 64 (2008) m1152–m1153; doi:10.1107/S1600536808024963

data_2219246
_publ_section_title
;
 Bis[tris(ethane-1,2-diamine)nickel(II)] octacyanidomolybdate(IV)
 dihydrate
;
_journal_coeditor_code           BR2077
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1152
_journal_page_last               m1153
_journal_paper_doi               10.1107/S1600536808024963
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C2 H8 N2)3]2 [Mo (C N)8], 2H2 O'
_chemical_formula_moiety         '2(C6 H24 N6 Ni 2+), C8 Mo N8 4-, 2(H2 O)'
_chemical_formula_sum            'C20 H52 Mo N20 Ni2 O2'
_chemical_formula_weight         818.18
_chemical_name_systematic
;
Bis[tris(ethane-1,2-diamine)nickel(II)] octacyanidomolybdate(IV) dihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 106.6830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1765(3)
_cell_length_b                   12.2178(2)
_cell_length_c                   15.8932(3)
_cell_measurement_reflns_used    4517
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      2.13
_cell_volume                     1892.89(7)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15991
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pale
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.923
_refine_ls_abs_structure_details 'Flack (1983), 2876 Friedel pairs'
_refine_ls_abs_structure_Flack   0.024(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6779
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0519
_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^)+(0.07P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                6292
_reflns_number_total             6779
_reflns_threshold_expression     I>\2s(I)
_cod_data_source_file            br2077.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2219246
_cod_database_fobs_code          2219246