A family of germanates constructed from Ge7clusters co-templated by metal complexes and organic/inorganic species
Ren, Xiaoyan; Pan, Qinhe; Liu, Jiancong; Li, Yi; Wang, Fuxiang; Li, Jiyang; Xu, Yan; Li, Li; CrystEngComm 16 (2014) 9545–; doi:10.1039/C4CE00671B

data_7217800
_publ_section_title
;
 A family of germanates constructed from Ge7clusters co-templated by metal
 complexes and organic/inorganic species
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              9545
_journal_paper_doi               10.1039/C4CE00671B
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety
'[C2H8NO]2 [Ni2 (C8N5H23)2 (C2N2H8)] [Ge7O14F3]2 H2O'
_chemical_formula_sum            'C22 H72 F6 Ge14 N14 Ni2 O31'
_chemical_formula_weight         2276.62
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-07-20 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8089(18)
_cell_length_b                   22.436(5)
_cell_length_c                   31.193(6)
_cell_measurement_temperature    293(2)
_cell_volume                     6165(2)
_computing_cell_refinement       Process-auto
_computing_data_collection       Process-auto
_computing_data_reduction        Process-auto
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXP-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            34855
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    7.419
_exptl_absorpt_correction_T_max  0.4026
_exptl_absorpt_correction_T_min  0.2134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
The remaining charge balancing organic species cations were disordered and assigned as eight protonated ethanolamine cations per unit cell, which were determined by TGA and elemental analysis. Then, the formula can be get as (NH3CH2CH2OH)2 [Ni2(TEPA)2(en)] [Ge7O14F3]2 H2O, with elemental analysis of C 11.61 (calcd wt%) 11.45 (found wt%), N 8.62 (calcd wt%) 8.86 (found wt%), N 3.19 (calcd wt%) 3.25 (found wt%). The contributions of these disordered protonated ethanolamine cations to the scattering values have been removed by using the PLATON SQUEEZE program.
;
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                5534
_reflns_number_total             6400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00671b2.cif
_cod_data_source_block           b_sqd
_cod_depositor_comments
'Adding full bibliography for 7217797--7217800.cif.'
_cod_original_sg_symbol_H-M      Pbcm
_cod_database_code               7217800
_platon_squeeze_void_probe_radius 1.20