[Ni(1,2-PDA)3]2(HOCH2CH2CH2NH3)3(H3O)2[Ge7O14X3]3(X= F, OH): A New 1D Germanate with 12-Ring Hexagonal Tubular Channels
Pan, Qinhe; Li, Jiyang; Ren, Xiaoyan; Wang, Zhuopeng; Li, Guanghua; Yu, Jihong; Xu, Ruren; Chemistry of Materials 20 (2008) 370–; doi:10.1021/cm702439v

data_4001102
_publ_section_title
;
 [Ni(1,2-PDA)3]2(HOCH2CH2CH2NH3)3(H3O)2[Ge7O14X3]3(X= F, OH): A New 1D
 Germanate with 12-Ring Hexagonal Tubular Channels
;
_journal_issue                   2
_journal_name_full               'Chemistry of Materials'
_journal_page_first              370
_journal_paper_doi               10.1021/cm702439v
_journal_volume                  20
_journal_year                    2008
_chemical_formula_moiety         'C27 H100.50 F4.50 Ge21 N15 Ni2 O51.50'
_chemical_formula_sum            'C27 H100.5 F4.5 Ge21 N15 Ni2 O51.5'
_chemical_formula_weight         3187.03
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   18.800(3)
_cell_length_b                   18.800(3)
_cell_length_c                   14.147(3)
_cell_measurement_reflns_used    3443
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.14
_cell_volume                     4330.2(13)
_computing_cell_refinement       Process-auto
_computing_data_collection       Process-auto
_computing_data_reduction        Process-auto
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'omega scan'
_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  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43665
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.14
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    7.699
_exptl_absorpt_correction_T_max  0.6781
_exptl_absorpt_correction_T_min  0.3748
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Process-auto
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.444
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal rod-shaped'
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.820
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3443
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0586P)^2^+24.9089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                2849
_reflns_number_total             3443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm702439v-file003.cif
_cod_data_source_block           JLG-4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Hexagonal' changed to 'hexagonal' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 
;
_cod_original_cell_volume        4330.2(12)
_cod_original_sg_symbol_Hall     -P6c
_cod_original_sg_symbol_H-M      P6(3)/m
_cod_original_formula_sum        'C27 H100.50 F4.50 Ge21 N15 Ni2 O51.50'
_cod_database_code               4001102