Supramolecular motifs and solvatomorphism within the compounds [M(bpy)3]2[NbO(C2O4)3]Cl·nH2O (M = Fe2+, Co2+, Ni2+, Cu2+ and Zn2+; n = 11, 12). Syntheses, structures and magnetic properties
Jurić, Marijana; Perić, Berislav; Brničević, Nevenka; Planinić, Pavica; Pajić, Damir; Zadro, Krešo; Giester, Gerald; Kaitner, Branko; Dalton Transactions  (2008) 742–754; doi:10.1039/b707937k

data_7003034
_publ_section_title
;
 Supramolecular motifs and solvatomorphism within the compounds
 [M(bpy)3]2[NbO(C2O4)3]Cl&#x00B7;nH2O (M = Fe2+, Co2+, Ni2+, Cu2+ and
 Zn2+; n = 11, 12). Syntheses, structures and magnetic properties
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              742
_journal_page_last               754
_journal_paper_doi               10.1039/b707937k
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C30 H24 N6 Ni), C6 Nb O13, 12(H2 O), Cl'
_chemical_formula_structural     '2(C30 H24 N6 Ni), C6 Nb O13, 12(H2 O), Cl'
_chemical_formula_sum            'C66 H72 Cl N12 Nb Ni2 O25'
_chemical_formula_weight         1679.14
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0580(10)
_cell_length_b                   22.039(2)
_cell_length_c                   22.398(2)
_cell_measurement_reflns_used    22608
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      3.40
_cell_volume                     7433.1(11)
_computing_cell_refinement       'DENZO-SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius Collect Software (Nonius, 1998)'
_computing_data_reduction        'DENZO-SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'PLATON (Spek, 2003), ORTEP-3, (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(3)
_diffrn_detector_area_resol_mean 18.4
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius-Kappa CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_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    0.0483
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22608
_diffrn_reflns_reduction_process
;
?
;
_diffrn_reflns_theta_full        30.49
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark pink'
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.487
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         22608
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                16952
_reflns_number_total             22608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b707937k.txt
_cod_data_source_block           V
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 
;
_cod_database_code               7003034