On the influence of the titanium source on the composition and structure of novel titanoniobates.
Dopta, Joanna; Grzanna, Sven; Näther, Christian; Bensch, Wolfgang; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15103–15113; doi:10.1039/c8dt02835d

data_7047668
_publ_section_title
;
 On the influence of the titanium source on the composition and structure
 of novel titanoniobates.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15103
_journal_page_last               15113
_journal_paper_doi               10.1039/c8dt02835d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         K+,3(NiC10H24N12)2+,1(TiNb9O28)7-,18(H2O)
_chemical_formula_sum            'C30 H108 K N12 Nb9 Ni3 O46 Ti'
_chemical_formula_weight         2472.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-09-14 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.847(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3130(6)
_cell_length_b                   19.1246(5)
_cell_length_c                   15.9741(4)
_cell_measurement_reflns_used    8279
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.005
_cell_measurement_theta_min      1.343
_cell_volume                     7594.9(3)
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_collection       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_molecular_graphics
'XP (Sheldrick, 2008) and Diamond (Brandenburg, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30337
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.005
_diffrn_reflns_theta_min         1.343
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.337
_exptl_absorpt_correction_T_max  0.7340
_exptl_absorpt_correction_T_min  0.6517
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5012
_exptl_crystal_size_max          0.1158
_exptl_crystal_size_mid          0.0934
_exptl_crystal_size_min          0.0785
_refine_diff_density_max         0.834
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.00026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         8279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+81.0076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7224
_reflns_number_total             8279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02835d2.cif
_cod_data_source_block           jo2633
_cod_depositor_comments
'Adding full bibliography for 7047668--7047670.cif.'
_cod_original_formula_sum        'C30 H108 K1 N12 Nb9 Ni3 O46 Ti'
_cod_database_code               7047668
_shelxl_version_number           2014-3
_shelx_res_checksum              19878