Three at a Time: Step by Step to Heterotermetallic Molecules.
Heidemann, Tim; Mathur, Sanjay; Inorganic chemistry 56 (2017) 234–240; doi:10.1021/acs.inorgchem.6b02069

data_4345127
_publ_section_title
;
 Three at a Time: Step by Step to Heterotermetallic Molecules.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              234
_journal_page_last               240
_journal_paper_doi               10.1021/acs.inorgchem.6b02069
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C54 H126 Ba2 I2 O18 Zr4'
_chemical_formula_sum            'C54 H126 Ba2 I2 O18 Zr4'
_chemical_formula_weight         1956.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 123.826(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1282(3)
_cell_length_b                   19.3448(5)
_cell_length_c                   21.0636(5)
_cell_measurement_reflns_used    55980
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.83
_cell_measurement_theta_min      1.98
_cell_volume                     4105.4(2)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'IPDS 2T (Stoe & Cie)'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60821
_diffrn_reflns_theta_full        26.83
_diffrn_reflns_theta_max         26.83
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    2.233
_exptl_absorpt_correction_T_max  0.7776
_exptl_absorpt_correction_T_min  0.4135
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The absorption correlation (X-RED; Stoe & Cie, 2001)
was performed after optimizing the crystal shape
using X-SHAPE (Stoe & Cie; 1999)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.763
_refine_diff_density_min         -1.695
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       'not measured'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         8589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0318P)^2^+6.3315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                7681
_reflns_number_total             8589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02069_si_002.cif
_cod_data_source_block           IBaZr2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        4105.38(18)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4345127