Crystal structure of μ-carbonato-bis[diaqua(N,N,N',N'- tetramethylethylenediamine)nickel(II)] perchlorate, [Ni(C6H16N2)(H2O)2(CO3)0.5]2(ClO4)2
Keiko Miyamoto; Ernst Horn; Yutaka Fukuda; Zeitschrift für Kristallographie - New Crystal Structures 224 (2009) 131–; doi:

data_8102412
_publ_section_title
;
 Crystal structure of \m-carbonato-bis[diaqua(N,N,N',N'-
 tetramethylethylenediamine)nickel(II)] perchlorate,
 [Ni(C6H16N2)(H2O)2(CO3)0.5]2(ClO4)2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              131
_journal_volume                  224
_journal_year                    2009
_chemical_formula_sum            'C40 H120 Cl4 N12 Ni6 O40'
_chemical_formula_weight         1903.54
_chemical_name_systematic
; 
\m-Carbonato-bis[diaqua(N,N,N',N'-tetramethylethylenediamine)
nickel(II)] perchlorate
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.684(2)
_cell_length_b                   19.076(3)
_cell_length_c                   6.2971(11)
_cell_measurement_reflns_used    2820
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      51.589
_cell_measurement_theta_min      5.514
_cell_volume                     1403.5(4)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w/\j 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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8068
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    2.294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemans, 2005)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .17
_exptl_crystal_size_min          .16
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.330
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876881'
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+1.0241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1073
_reflns_number_gt                2631
_reflns_number_total             2991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2517.cff
_cod_data_source_block           ehfy621s
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' 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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2
_cod_database_code               8102412
_exptl_absorpt_correction_t_min/max 0.69