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_7048773
_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 O22 Si4 Zr2, 1.8(C7 H8), 0.2(C H2 Cl2)'
_chemical_formula_sum            'C108.8 H134.8 Ca2 Cl0.4 O22 Si4 Zr2'
_chemical_formula_weight         2183.71
_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   geom
_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                103.64(4)
_cell_angle_beta                 95.93(4)
_cell_angle_gamma                113.43(4)
_cell_formula_units_Z            1
_cell_length_a                   11.421(3)
_cell_length_b                   14.263(4)
_cell_length_c                   19.107(5)
_cell_measurement_reflns_used    5552
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      25.9999
_cell_measurement_theta_min      2.9340
_cell_volume                     2706.7(18)
_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      101(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'KUMA KM4 CCD \k-geometry diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.1253
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21235
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.057
_diffrn_reflns_theta_min         2.940
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.933
_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            colorless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             1146
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.584
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         10648
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0628P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7403
_reflns_number_total             10648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03796e2.cif
_cod_data_source_block           7x1'8C7H8x0'2CH2Cl2
_cod_depositor_comments
'Adding full bibliography for 7048765--7048774.cif.'
_cod_original_formula_sum        'C108.80 H134.80 Ca2 Cl0.40 O22 Si4 Zr2'
_cod_database_code               7048773
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.968
_shelx_res_checksum              41800