Zn and Fe Complexes Containing a Redox Active Macrocyclic Biquinazoline Ligand
Priyabrata Banerjee; Anna Company; Thomas Weyhermüller; Eckhard Bill; Corinna R. Hess; Inorganic Chemistry 48 (2009) 2944–2955; doi:10.1021/ic8020172

data_4301798
_publ_section_title
;
Zn and Fe Complexes Containing a Redox Active Macrocyclic Biquinazoline
Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2944
_journal_page_last               2955
_journal_paper_doi               10.1021/ic8020172
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'[C33 H33 Cl N8 Zn], 0.6 (C H2 Cl2), 0.4 ( H2 O)'
_chemical_formula_sum            'C33.6 H35 Cl2.2 N8 O0.4 Zn'
_chemical_formula_weight         700.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 110.843(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1513(4)
_cell_length_b                   21.3607(9)
_cell_length_c                   15.4174(6)
_cell_measurement_temperature    100(2)
_cell_volume                     3432.1(2)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
'1355 images at 0.5 deg. stepwise rotation in omega and phi, 40 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
'rotating anode, 50 kV, 40 mA, Multi-Layer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57527
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  0.9132
_exptl_absorpt_correction_T_min  0.6271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS-2006/1'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             1453
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         9982
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+4.8798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1317
_reflns_number_gt                7352
_reflns_number_total             9982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8020172_si_002_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C33.60 H35 Cl2.20 N8 O0.40 Zn'
_cod_database_code               4301798