Synthesis and Characterization of Benzotriazole or Benzoxazole Phenoxide Ligands Supported Nb and Ta Metal Complexes and their Application for the Synthesis of Hyperbranched Polyglycerols by Ring-Opening Polymerisation of Glycidol
pappuru, sreenath; Chakraborty, Debashis; V, Ramkumar; Dalton Transactions  (2017) –; doi:10.1039/C7DT02839C

data_7044718
_publ_section_title
;
 Synthesis and Characterization of Benzotriazole or Benzoxazole Phenoxide
 Ligands Supported Nb and Ta Metal Complexes and their Application for the
 Synthesis of Hyperbranched Polyglycerols by Ring-Opening Polymerisation
 of Glycidol
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT02839C
_journal_year                    2017
_chemical_formula_sum            'C52 H40 Cl8 N12 Nb4 O8'
_chemical_formula_weight         1616.20
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c'
_symmetry_space_group_name_Hall  '-P 4a 2bc'
_symmetry_space_group_name_H-M   'P 4/n n c :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-11-01 deposited with the CCDC.
2017-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.028(4)
_cell_length_b                   20.028(4)
_cell_length_c                   20.966(5)
_cell_measurement_reflns_used    880
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.18
_cell_measurement_theta_min      2.42
_cell_volume                     8410(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1824
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29020
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.036
_diffrn_reflns_theta_max         20.036
_diffrn_reflns_theta_min         1.406
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.099
_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     191
_refine_ls_number_reflns         1985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0859P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1353
_reflns_number_total             1985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02839c2.cif
_cod_data_source_block           tri-nb-sq
_cod_original_cell_volume        8410(4)
_cod_database_code               7044718
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.886
_shelx_estimated_absorpt_t_max   0.922
_shelx_res_checksum              16260