An unsupported metal hydroxide for the design of molecular mu-oxo bridged heterobimetallic complexes
A. J. Falzone; J. Nguyen; W. W. Weare; R. D. Sommer; P. D. Boyleb; Chem.Commun. 50 (2014) 2139–; doi:10.1039/c3cc49066a

data_7111986
_publ_section_title
;
 An unsupported metal hydroxide for the design of molecular mu-oxo bridged
 heterobimetallic complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              2139
_journal_paper_doi               10.1039/c3cc49066a
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C115 H77 B2 Cl4 Cr F48 N6 O4 Ti'
_chemical_formula_weight         2782.14
_chemical_name_common            'CrOTi Falzone'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90.4300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4112(3)
_cell_length_b                   18.3529(5)
_cell_length_c                   46.9774(11)
_cell_measurement_reflns_used    9785
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      26.1805
_cell_measurement_theta_min      2.2194
_cell_volume                     11562.4(5)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            139961
_diffrn_reflns_theta_full        26.56
_diffrn_reflns_theta_max         26.56
_diffrn_reflns_theta_min         1.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            pink-orange
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             5588
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.692
_refine_diff_density_min         -1.725
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1684
_refine_ls_number_reflns         23703
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0904P)^2^+36.2499P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1920
_reflns_number_gt                19058
_reflns_number_total             23703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3cc49066a.txt
_cod_data_source_block           I
_cod_database_code               7111986
_shelx_res_checksum              80683
_shelx_hkl_checksum              27938