Synthesis, Complexation, and Coordination Oligomerization of 1,8-Pyrazine-Capped 5,12-Dioxocyclams
Louis S. Hegedus; Michael J. Sundermann; Peter K. Dorhout; Inorganic Chemistry 42 (2003) 4346–4354; doi:10.1021/ic030090j

data_4313862
_publ_section_title
;
 Synthesis, Complexation, and Coordination Oligomerization of
 1,8-Pyrazine-Capped 5,12-Dioxocyclams
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4346
_journal_page_last               4354
_journal_paper_doi               10.1021/ic030090j
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C34 H44 N8 O4'
_chemical_formula_weight         628.77
_chemical_name_common            'Pyrazine Capped Copper Cyclam'
_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                 90.000(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.542(7)
_cell_length_b                   13.601(9)
_cell_length_c                   23.271(16)
_cell_measurement_reflns_used    5169
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.96
_cell_measurement_theta_min      1.09
_cell_volume                     3337(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  '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  0.0723
_diffrn_reflns_av_sigmaI/netI    0.0962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15354
_diffrn_reflns_theta_full        23.48
_diffrn_reflns_theta_max         23.48
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow/oran
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubes
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.80
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0801
_reflns_number_gt                2668
_reflns_number_total             4823
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030090j_3.cif
_cod_data_source_block           Complex5a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313862