Synthesis and Characterization of Group 4 Trianionic ONO3‒ Pincer-Type Ligand Complexes and a Rare Case of Through-Space 19F‒19F Coupling
Nadif, Soufiane S.; Pedziwiatr, Jakub; Ghiviriga, Ion; Abboud, Khalil A.; Veige, Adam S.; Organometallics 34 (2015) 1107–; doi:10.1021/acs.organomet.5b00036

data_4087378
_publ_section_title
;
 Synthesis and Characterization of Group 4 Trianionic ONO3-- Pincer-Type
 Ligand Complexes and a Rare Case of Through-Space 19F--19F Coupling
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1107
_journal_paper_doi               10.1021/acs.organomet.5b00036
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C33 H31 F12 N O3 Ti'
_chemical_formula_weight         765.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-12-22 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 94.549(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.253(4)
_cell_length_b                   41.867(16)
_cell_length_c                   17.033(7)
_cell_measurement_reflns_used    3719
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     6578(5)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2552
_diffrn_reflns_av_unetI/netI     0.2130
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54007
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.544
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_correction_T_min  0.9515
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_description       plates
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         11557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.2014
_refine_ls_R_factor_gt           0.0965
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0743P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5298
_reflns_number_total             11557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00036_si_002.cif
_cod_data_source_block           souf9
_cod_original_cell_volume        6578(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4087378
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.995
_shelxl_version_number           2013-3
_shelx_res_checksum              44928
_shelx_hkl_checksum              15992