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_7224381
_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_sum            'C48 H68 Cl4 N8 O6 Zr2'
_chemical_formula_weight         1177.34
_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   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-20 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                106.403(6)
_cell_angle_beta                 91.013(7)
_cell_angle_gamma                108.188(6)
_cell_formula_units_Z            1
_cell_length_a                   9.9338(13)
_cell_length_b                   11.1209(15)
_cell_length_c                   14.560(2)
_cell_measurement_reflns_used    6834
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2.8
_cell_volume                     1456.0(3)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15810
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.023
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruer, 1999)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4933
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0764P)^2^+2.2679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4096
_reflns_number_total             4933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra26721h2.cif
_cod_data_source_block           DMNZR
_cod_original_cell_volume        1456.0(4)
_cod_database_code               7224381
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_checksum              2453