Transformation of molecular compounds with Ba(Sr)/Al/Si and Ca(Sr, Ba)/Ti(Zr, Hf)/Si heteroelements as new efficient route to metal silicate materials.
Petrus, R.; Drąg-Jarząbek, A; Utko, J.; Lis, T.; Sobota, P.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4283–4298; doi:10.1039/c8dt03796e

data_7048770
_publ_section_title
;
 Transformation of molecular compounds with Ba(Sr)/Al/Si and Ca(Sr,
 Ba)/Ti(Zr, Hf)/Si heteroelements as new efficient route to metal silicate
 materials.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4283
_journal_page_last               4298
_journal_paper_doi               10.1039/c8dt03796e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C96 H120 Ca2 Hf2 O22 Si4, 2(C7 H8), 2(H2 O)'
_chemical_formula_sum            'C110 H140 Ca2 Hf2 O24 Si4'
_chemical_formula_weight         2395.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-01-09 deposited with the CCDC.
2019-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                100.03(2)
_cell_angle_beta                 102.58(3)
_cell_angle_gamma                112.84(3)
_cell_formula_units_Z            1
_cell_length_a                   11.394(4)
_cell_length_b                   14.120(4)
_cell_length_c                   19.167(5)
_cell_measurement_reflns_used    8935
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      30.6772
_cell_measurement_theta_min      2.8702
_cell_volume                     2656.4(17)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'DIAMOND  (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Xcalibur Ruby'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
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_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17022
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.499
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.876
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_T_max  0.785
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_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       needle
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         3.660
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         9682
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+8.9206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8831
_reflns_number_total             9682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03796e2.cif
_cod_data_source_block           8x2C7H8x2H2O
_cod_depositor_comments
'Adding full bibliography for 7048765--7048774.cif.'
_cod_database_code               7048770
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.603
_shelx_estimated_absorpt_t_max   0.766
_shelx_res_checksum              77278