Imino phenoxide complexes of group 4 metals: synthesis, structural characterization and polymerization studies
Saha, Tanmoy Kumar; Mandal, Mrinmay; Chakraborty, Debashis; Ramkumar, Venkatachalam; New Journal of Chemistry 37 (2013) 949–; doi:10.1039/c3nj40916c

data_7053032
_publ_section_title
;
 Imino phenoxide complexes of group 4 metals: synthesis, structural
 characterization and polymerization studies
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              949
_journal_paper_doi               10.1039/c3nj40916c
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         ' C44 H54 Br4 N2 O4 Zr, C7 H8 '
_chemical_formula_sum            'C51 H62 Br4 N2 O4 Zr'
_chemical_formula_weight         1177.89
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.119(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.9206(11)
_cell_length_b                   10.1128(5)
_cell_length_c                   23.1925(12)
_cell_measurement_reflns_used    6533
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      2.43
_cell_volume                     5112.0(4)
_computing_cell_refinement       APEXII,Bruker,2004
_computing_data_collection       APEXII,Bruker,2004
_computing_data_reduction        SAINT,Bruker,2004
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEXII 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_R_equivalents  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28555
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    3.385
_exptl_absorpt_correction_T_max  0.6307
_exptl_absorpt_correction_T_min  0.4849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.349
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.112
_refine_ls_extinction_coef       0.00006(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         9436
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+4.8607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                6236
_reflns_number_total             9436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj40916c.txt
_cod_data_source_block           Zr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7053032