Two Open-Framework Germanates with Nickel Complexes Incorporated into the Framework
Shiliang Huang; Kirsten Christensen; Maxim V. Peskov; Sihai Yang; Kuo Li; Xiaodong Zou; Junliang Sun; Inorganic Chemistry 50 (2011) 9921–9923; doi:10.1021/ic2013478

data_4326525
_publ_section_title
;
 Two Open-Framework Germanates with Nickel Complexes Incorporated into the
 Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9921
_journal_page_last               9923
_journal_paper_doi               10.1021/ic2013478
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'C4 H21.87 Ge22 N4 Ni O51, 2(C2 H10 N2), 2(C2 H9 N2), 9.04(H2 O)'
_chemical_formula_sum            'C12 H77.95 Ge22 N12 Ni O60.04'
_chemical_formula_weight         3007.14
_chemical_name_common            SUT-1b
_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                90.00
_cell_angle_beta                 98.228(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8907(2)
_cell_length_b                   30.9833(5)
_cell_length_c                   20.7890(5)
_cell_measurement_reflns_used    19254
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.6
_cell_measurement_theta_min      1.2
_cell_volume                     6942.6(2)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
        (compiled Dec  8 2009,17:31:18)
;
_computing_data_collection
;
        CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
        (compiled Dec  8 2009,17:31:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            64269
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    8.754
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            lilac
_exptl_crystal_density_diffrn    2.877
_exptl_crystal_description       'Plate Crystal'
_exptl_crystal_F_000             5785
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.555
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         13967
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0467P)^2^+28.5173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                11735
_reflns_number_total             13967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2013478_si_004_2.cif
_cod_data_source_block           sut-2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4326525