Group 4 alkoxide complexes containing [NNO]-type scaffold: synthesis, structural characterization and polymerization studies
Mandal, Dipa; Chakraborty, Debashis; Ramkumar, Venkatachalam; Chand, Dillip Kumar; RSC Adv. 6 (2016) 21706–; doi:10.1039/C5RA26721H

data_7224382
_publ_section_title
;
 Group 4 alkoxide complexes containing [NNO]-type scaffold: synthesis,
 structural characterization and polymerization studies
;
_journal_issue                   26
_journal_name_full               'RSC Adv.'
_journal_page_first              21706
_journal_paper_doi               10.1039/C5RA26721H
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C44 H60 Hf2 N8 O6, 2(C H Cl3)'
_chemical_formula_sum            'C46 H62 Cl6 Hf2 N8 O6'
_chemical_formula_weight         1392.7
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-11-20 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                108.4480(10)
_cell_angle_beta                 90.6828(11)
_cell_angle_gamma                101.2321(10)
_cell_formula_units_Z            1
_cell_length_a                   9.6702(3)
_cell_length_b                   10.9556(3)
_cell_length_c                   14.5845(4)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.51
_cell_volume                     1433.15(7)
_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 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.993
_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  0.0173
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_laue_measured_fraction_full 0.965
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21435
_diffrn_reflns_point_group_measured_fraction_full 0.793
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.004
_exptl_absorpt_coefficient_mu    3.948
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2012)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       Block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
; 
 Flack x determined using 2962 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.497(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         8227
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+1.5102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0490
_reflns_Friedel_coverage         0.644
_reflns_friedel_fraction_full    0.621
_reflns_friedel_fraction_max     0.639
_reflns_number_gt                7715
_reflns_number_total             8227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra26721h2.cif
_cod_data_source_block           dmn
_cod_database_code               7224382
_shelx_estimated_absorpt_t_min   0.477
_shelx_estimated_absorpt_t_max   0.694
_shelxl_version_number           2014-3
_shelx_res_checksum              46770