Extending the Family of Titanium Heterometallic-oxo-alkoxy Cages
Salvador Eslava; Benjamin P. R. Goodwill; Mary McPartlin; Dominic S. Wright; Inorganic Chemistry 50 (2011) 5655–5662; doi:10.1021/ic200350j

data_4325407
_publ_contact_author_address
;
 University of Cambridge
 Department of Chemistry   
 Lensfield Road
 Cambridge
 CB2 1EW
 England   
;
_publ_contact_author_email       se296@cam.ac.uk
_publ_contact_author_name        'S. Eslava'
_publ_section_title
;
 Extending the Family of Titanium Heterometallic-oxo-alkoxy Cages
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5655
_journal_page_last               5662
_journal_paper_doi               10.1021/ic200350j
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C30 H75 Cl O16 Zn Zr4'
_chemical_formula_sum            'C30 H75 Cl O16 Zn Zr4'
_chemical_formula_weight         1157.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
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_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                 117.790(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.1264(3)
_cell_length_b                   11.2806(2)
_cell_length_c                   22.5715(4)
_cell_measurement_reflns_used    64539
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.02
_cell_volume                     4984.03(15)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0483
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34097
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         3.55
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
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_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.608
_refine_diff_density_min         -1.607
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.555
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         8966
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      3.552
_refine_ls_R_factor_all          0.1718
_refine_ls_R_factor_gt           0.1567
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4262
_refine_ls_wR_factor_ref         0.4418
_reflns_number_gt                7763
_reflns_number_total             8966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200350j_si_001_6.cif
_cod_data_source_block           6
_cod_original_cell_volume        4984.03(14)
_cod_database_code               4325407