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_7019046
_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_moiety         '2 C35 H47 Cl Cu N6, C4 H10 O, 0.6 C2 H3 N'
_chemical_formula_sum            'C75.2 H105.8 Cl2 Cu2 N12.6 O'
_chemical_formula_weight         1400.30
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9395(3)
_cell_length_b                   16.1910(3)
_cell_length_c                   26.7675(5)
_cell_measurement_reflns_used    28634
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.7261
_cell_measurement_theta_min      2.6063
_cell_volume                     7341.5(2)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2011)'
_computing_molecular_graphics    'Mercury 2.0 (Bruno et al, 2002)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008) and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1992)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57040
_diffrn_reflns_theta_full        75.91
_diffrn_reflns_theta_max         75.91
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  0.8949
_exptl_absorpt_correction_T_min  0.6130
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2981
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.090
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 7243 Friedel pairs'
_refine_ls_abs_structure_Flack   0.488(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         14997
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0622P)^2^+7.9680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                14290
_reflns_number_total             14997
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2dt30539a.txt
_cod_data_source_block           CuClH2L1
_cod_original_formula_sum        'C75.20 H105.80 Cl2 Cu2 N12.60 O'
_cod_database_code               7019046