Influence of the [2.1.1]-(2,6)-Pyridinophane Macrocycle Ring Size Constraint on the Structure and Reactivity of Copper Complexes
A. N. Vedernikov; M. Pink; K. G. Caulton; Inorganic Chemistry 43 (2004) 4300–4305; doi:10.1021/ic049886o

data_4311308
_publ_section_title
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 Influence of the [2.1.1]-(2,6)-Pyridinophane Macrocycle Ring Size
 Constraint on the Structure and Reactivity of Copper Complexes
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4300
_journal_page_last               4305
_journal_paper_doi               10.1021/ic049886o
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C38 H36 Cu2 N6 O2, C H2 Cl2, 2(C F3 O3 S)'
_chemical_formula_sum            'C41 H38 Cl2 Cu2 F6 N6 O8 S2'
_chemical_formula_weight         1118.87
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.677(2)
_cell_angle_beta                 69.113(2)
_cell_angle_gamma                74.624(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9327(9)
_cell_length_b                   10.6687(10)
_cell_length_c                   11.3605(10)
_cell_measurement_reflns_used    2832
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.4
_cell_volume                     1084.33(17)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'XTEL (local library)'
_computing_publication_material  'XCIF (Bruker, 1999), XTEL (local library)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
'0.30 degree frames measured for 80 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       \w-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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12569
_diffrn_reflns_theta_full        25.51
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    1.288
_exptl_absorpt_correction_T_max  0.9624
_exptl_absorpt_correction_T_min  0.8608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing (1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3969
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+2.4017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                2962
_reflns_number_total             3969
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049886osi20040128_092440.cif
_cod_data_source_block           03080
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4311308