Directed secondary interactions in transition metal complexes of tripodal pyrrole imine and amide ligands
Hart, John S.; Nichol, Gary S.; Love, Jason B.; Dalton Transactions 41 (2012) 5785–; doi:10.1039/c2dt30539a

data_7019047
_publ_section_title
;
 Directed secondary interactions in transition metal complexes of tripodal
 pyrrole imine and amide ligands
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              5785
_journal_paper_doi               10.1039/c2dt30539a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C32 H45 N9 O5 Ti'
_chemical_formula_weight         683.67
_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                 112.407(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.704(10)
_cell_length_b                   35.30(3)
_cell_length_c                   9.483(12)
_cell_measurement_reflns_used    5234
_cell_measurement_temperature    160
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     3622(6)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 rc12 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc12 (Rigaku, 2009)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 rc12 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      160
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device       'XtaLABmini: Fixed Chi 2 circle'
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1237
_diffrn_reflns_av_sigmaI/netI    0.1103
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19852
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_T_max  0.9449
_exptl_absorpt_correction_T_min  0.9449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear, Rigaku 2010'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0871
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+2.6439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.2089
_reflns_number_gt                4080
_reflns_number_total             6022
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2dt30539a.txt
_cod_data_source_block           '[Ti(OiPr)2(H4L2b)]'
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3622(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7019047