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_7055934
_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 H90 Cl10 N20 Ti'
_chemical_formula_weight         1181.65
_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                82.059(8)
_cell_angle_beta                 76.615(7)
_cell_angle_gamma                78.133(7)
_cell_formula_units_Z            1
_cell_length_a                   8.6586(9)
_cell_length_b                   13.0597(14)
_cell_length_c                   14.2197(15)
_cell_measurement_reflns_used    3079
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3255
_cell_measurement_theta_min      2.2505
_cell_volume                     1523.9(3)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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_unetI/netI     0.0887
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5269
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.479
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.9404
_exptl_absorpt_correction_T_min  0.9125
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1230 (selected reflections only, before parameter refinement)
 R(int) =  0.0795 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       plate
_exptl_crystal_F_000             626
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1170
_refine_ls_R_factor_gt           0.0869
_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^)+(0.1187P)^2^+3.5854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2260
_refine_ls_wR_factor_ref         0.2456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3802
_reflns_number_total             5269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03489f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7055933--7055935.cif.'
_cod_database_code               7055934
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              52342