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_4313860
_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            'C32 H50 Cu N6 O10 Rh'
_chemical_formula_weight         845.23
_chemical_name_common            'Bis Copper Bis Rhodium'
_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                96.406(6)
_cell_angle_beta                 93.866(6)
_cell_angle_gamma                104.369(6)
_cell_formula_units_Z            2
_cell_length_a                   9.533(3)
_cell_length_b                   14.048(5)
_cell_length_c                   14.153(5)
_cell_measurement_reflns_used    5223
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      23.27
_cell_measurement_theta_min      3.10
_cell_volume                     1815.7(11)
_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      183(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0754
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11570
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green/brown
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0042(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         5223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                3754
_reflns_number_total             5223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030090j_1.cif
_cod_data_source_block           complex8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_original_cell_volume        1815.7(10)
_cod_database_code               4313860