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_4087377
_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            'C25 H23 F12 N O3 Ti'
_chemical_formula_weight         661.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2013-11-05 # Formatted by publCIF

;
_cell_angle_alpha                84.0275(13)
_cell_angle_beta                 89.6253(13)
_cell_angle_gamma                71.6678(13)
_cell_formula_units_Z            2
_cell_length_a                   8.7650(7)
_cell_length_b                   11.8664(9)
_cell_length_c                   13.6840(11)
_cell_measurement_reflns_used    6855
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     1343.18(18)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20310
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.497
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.9793
_exptl_absorpt_correction_T_min  0.9476
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       plates
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6165
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0620P)^2^+0.8228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4686
_reflns_number_total             6165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00036_si_002.cif
_cod_data_source_block           souf4
_cod_database_code               4087377
_publcif_datablock.id            {7d04f567-9671-45c1-bbaa-a26afaae4489}
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.970
_shelxl_version_number           2013-3
_shelx_res_checksum              12950
_shelx_hkl_checksum              2370
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n