Stereoselective Association of Binuclear Metallacycles in Coordination Polymers
Andrei N. Khlobystov; Matthew T. Brett; Alexander J. Blake; Neil R. Champness; Peter M. W. Gill; Darragh P. O'Neill; Simon J. Teat; Claire Wilson; Martin Schröder; Journal of the American Chemical Society 125 (2003) 6753–6761; doi:10.1021/ja029048y

data_4113779
_publ_contact_author_address
;
  School of Chemistry
  The University of Nottingham
  University Park
  Nottingham  NG7 2RD
  England
;
_publ_contact_author_email       A.J.Blake@nottingham.ac.uk
_publ_contact_author_fax         '0115 951 3563'
_publ_contact_author_name        'Dr A.J. Blake'
_publ_contact_author_phone       '0115 951 3488'
_publ_section_title
;
 Stereoselective Association of Binuclear Metallacycles in Coordination
 Polymers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6753
_journal_page_last               6761
_journal_paper_doi               10.1021/ja029048y
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C18 H12 N2 Cd 2+, 2(N O3 -), C2 H3 N'
_chemical_formula_sum            'C20 H15 Cd N5 O6'
_chemical_formula_weight         533.77
_chemical_name_common            Cd(NO3)2*Pyyne
_chemical_name_systematic
; 
 1(4-Pyridyl)-4(2-pyridylethynyl)benzene Cadmium bisnitrate complex 
 acetonitrile solvate 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens
'Me-group from delta-F synthesis, others placed geometrically'
_atom_sites_solution_primary     'Patterson method'
_atom_sites_solution_secondary   'difference Fourier method'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.583(5)
_cell_length_b                   8.1430(16)
_cell_length_c                   21.270(4)
_cell_measurement_reflns_used    958
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      3.15
_cell_volume                     4098.4(17)
_computing_cell_refinement       'SAINT version 6.02a (Bruker, 2000)'
_computing_data_collection       'SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL/PC version 5.03 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_sigmaI/netI    0.031
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17871
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  10
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.497
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       column
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.32
_refine_diff_density_min         -0.40
_refine_diff_density_rms         0.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment
'rigid rotator for Me-group, riding model for others'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4928
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.051P)^2^+4.524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                4030
_reflns_number_total             4928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029048ysi20021022_034217_5.cif
_cod_data_source_block           (5)
_cod_original_cell_volume        4098.3(14)
_cod_database_code               4113779