β-Nitro Derivatives of Germanium(IV) Corrolates
Marco Mastroianni; Weihua Zhu; Manuela Stefanelli; Sara Nardis; Frank R. Fronczek; Kevin M. Smith; Zhongping Ou; Karl M. Kadish; Roberto Paolesse; Inorganic Chemistry 47 (2008) 11680–11687; doi:10.1021/ic801421a

data_4306593
_publ_section_title
;
\b-Nitro Derivatives of Germanium(IV) Corrolates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11680
_journal_page_last               11687
_journal_paper_doi               10.1021/ic801421a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C74 H42 Ge2 N12 O9, 2(C H Cl3)'
_chemical_formula_sum            'C76 H44 Cl6 Ge2 N12 O9'
_chemical_formula_weight         1627.11
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
_cell_angle_beta                 94.528(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.634(2)
_cell_length_b                   16.1855(15)
_cell_length_c                   23.728(4)
_cell_measurement_reflns_used    13650
_cell_measurement_temperature    90
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.5
_cell_volume                     7134.0(16)
_computing_cell_refinement
'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare  et al., 1999)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' \w and \f 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  0.046
_diffrn_reflns_av_sigmaI/netI    0.0698
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            66866
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         26.4
_diffrn_reflns_theta_min         2.6
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo & Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark blue-green'
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.53
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         14509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.078
_refine_ls_R_factor_gt           0.049
_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^)+(0.0737P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.124
_refine_ls_wR_factor_ref         0.134
_reflns_number_gt                10171
_reflns_number_total             14509
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic801421a_si_002.cif
_cod_data_source_block
;
;
_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 
;
_cod_original_cell_volume        7134.0(15)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4306593