Synthesis and Characterization of Mixed-Metal Aryloxo-Organometallic Precursors for Oxide‒Ceramic Materials
John, Łukasz; Utko, Józef; Szafert, Sławomir; Jerzykiewicz, Lucjan B.; Kȩpiński, Leszek; Sobota, Piotr; Chemistry of Materials 20 (2008) 4231–4239; doi:10.1021/cm702262n

data_4001100
_publ_section_title
;
 Synthesis and Characterization of Mixed-Metal Aryloxo-Organometallic
 Precursors for Oxide--Ceramic Materials
;
_journal_coden_ASTM              CMATEX
_journal_issue                   13
_journal_name_full               'Chemistry of Materials'
_journal_page_first              4231
_journal_page_last               4239
_journal_paper_doi               10.1021/cm702262n
_journal_volume                  20
_journal_year                    2008
_chemical_formula_moiety         'C44 H54 Ba O8 Zn2'
_chemical_formula_sum            'C44 H54 Ba O8 Zn2'
_chemical_formula_weight         978.95
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.19(4)
_cell_angle_beta                 82.22(5)
_cell_angle_gamma                70.33(5)
_cell_formula_units_Z            2
_cell_length_a                   10.508(5)
_cell_length_b                   11.444(5)
_cell_length_c                   19.927(5)
_cell_measurement_reflns_used    8621
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      3
_cell_volume                     2234.4(17)
_computing_cell_refinement       'Oxford Diffraion software, CrystAlis 1.171'
_computing_data_collection       'Oxford Diffraion software, CrystAlis 1.171'
_computing_data_reduction        'Oxford Diffraion software, CrystAlis 1.171'
_computing_molecular_graphics    'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_publication_material  'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_structure_refinement  'SHELXTL-NT V5.1, Bruker AXS 1999'
_computing_structure_solution    'SHELXTL-NT V5.1, Bruker AXS 1999'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Kuma KM4CCD kappa-axis diffractometer'
_diffrn_measurement_method       \w
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27794
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    1.984
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Oxford Diffraion software, CrystAlis 1.171'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillars
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         10605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0307P)^2^+2.4869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                9337
_reflns_number_total             10605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm702262n-file.004.cif
_cod_data_source_block           for_complex_4_john14an
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

 Updated bibliographic information.

 Antanas Vaitkus,
 2019-09-24
;
_cod_database_code               4001100