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_7055935
_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            'C38 H74 Cl4 Hf4 N6 O18'
_chemical_formula_weight         1758.79
_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
_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                90
_cell_angle_beta                 102.888(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5959(12)
_cell_length_b                   18.794(2)
_cell_length_c                   14.5380(16)
_cell_measurement_reflns_used    8312
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.859
_cell_measurement_theta_min      2.309
_cell_volume                     3088.5(6)
_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    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CMOS area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28411
_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         25.999
_diffrn_reflns_theta_min         1.800
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.935
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.3939
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1339 (selected reflections only, before parameter refinement)
 R(int) =  0.0844(selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       cube
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         3.759
_refine_diff_density_min         -1.917
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6078
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0919P)^2^+20.1428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1701
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4346
_reflns_number_total             6078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03489f2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7055933--7055935.cif.'
_cod_database_code               7055935
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.368
_shelx_estimated_absorpt_t_max   0.443
_shelx_res_checksum              24309
_shelx_fab_checksum              76273