Synthesis and Structural Characterization of [Na2M(C5O5)2(H2O)2].4H2O (M = NiII, CuII)
Chih-Chieh Wang; Cheng-Han Yang; Gene-Hsiang Lee; Inorganic Chemistry 41 (2002) 1015–1018; doi:10.1021/ic0108538

data_4317565
_publ_section_title
;
 Synthesis and Structural Characterization of [Na2M(C5O5)2(H2O)2].4H2O (M
 = NiII, CuII)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1015
_journal_page_last               1018
_journal_paper_doi               10.1021/ic0108538
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C10 H12 Na2 Ni O16'
_chemical_formula_weight         492.89
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                100.54(2)
_cell_angle_beta                 111.74(2)
_cell_angle_gamma                99.622(15)
_cell_formula_units_Z            1
_cell_length_a                   6.9223(14)
_cell_length_b                   7.9382(13)
_cell_length_c                   8.703(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      16.38
_cell_measurement_theta_min      7.36
_cell_volume                     422.03(17)
_computing_cell_refinement       'Nonius CAD4'
_computing_data_collection       'Nonius CAD4'
_computing_data_reduction        'NRCSDP DATRD2'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       '\w--2\q 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
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_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.290
_exptl_absorpt_correction_T_max  0.7882
_exptl_absorpt_correction_T_min  0.6913
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             250
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.110
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_refine_ls_number_reflns         2454
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_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_obs          0.0250
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0703
_refine_ls_wR_factor_obs         0.0683
_reflns_number_observed          2182
_reflns_number_total             2454
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0108538_1.cif
_cod_data_source_block           ic7528
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

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

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0795P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.0795P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        422.00(14)
_cod_database_code               4317565