Synthesis and structural characterization of mixed halide‒N,N-diethylcarbamates of group 4 metals, including a case of unusual tetrahydrofuran activation
Bortoluzzi, Marco; Bresciani, Giulio; Marchetti, Fabio; Pampaloni, Guido; Zacchini, Stefano; New J. Chem. 41 (2017) 1781–; doi:10.1039/C6NJ03489F

data_7055933
_publ_section_title
;
 Synthesis and structural characterization of mixed
 halide--N,N-diethylcarbamates of group 4 metals, including a case of
 unusual tetrahydrofuran activation
;
_journal_issue                   4
_journal_name_full               'New J. Chem.'
_journal_page_first              1781
_journal_paper_doi               10.1039/C6NJ03489F
_journal_volume                  41
_journal_year                    2017
_chemical_formula_sum            'C34 H68 Cl14 N6 O12 Ti3'
_chemical_formula_weight         1392.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-12-27 deposited with the CCDC.
2017-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                106.064(5)
_cell_angle_beta                 102.815(5)
_cell_angle_gamma                104.401(4)
_cell_formula_units_Z            1
_cell_length_a                   10.7343(6)
_cell_length_b                   11.1683(6)
_cell_length_c                   14.4997(12)
_cell_measurement_reflns_used    4664
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.9815
_cell_measurement_theta_min      2.1535
_cell_volume                     1537.03(19)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0753
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22419
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.538
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.9030
_exptl_absorpt_correction_T_min  0.8510
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1045 (selected reflections only, before parameter refinement)
 R(int) =  0.0625 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       needle
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.7047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4044
_reflns_number_total             6032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03489f2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7055933--7055935.cif.'
_cod_original_cell_volume        1537.03(18)
_cod_database_code               7055933
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.903
_shelx_res_checksum              41145