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_4113775
_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         'C33 H27 N5 O6 Cd, 2(C2 H3 N)'
_chemical_formula_sum            'C37 H33 Cd N7 O6'
_chemical_formula_weight         784.10
_chemical_name_common            3PhPy*Cd(NO3)2
_chemical_name_systematic
; 
 Bis(nitrato-O,O)tris(4-phenylpyridine)cadmium(II) bis(acetonitrile solvate) 
;
_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
'aromatic placed geometrically, others from delta-F synthesis'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier method'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.780(2)
_cell_angle_beta                 95.372(2)
_cell_angle_gamma                112.184(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8471(7)
_cell_length_b                   13.0727(7)
_cell_length_c                   13.0765(7)
_cell_measurement_reflns_used    6967
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      2.35
_cell_volume                     1780.87(18)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART version 5.054 (Bruker, 1998)'
_computing_data_reduction        'SAINT version 6.01 (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL/PC version 5.03 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL97; PLATON (Spek, 2002)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'Bruker SMART1000 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  0.016
_diffrn_reflns_av_sigmaI/netI    0.016
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17801
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  10
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.36
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment
'riding model for aromatic H, rigid rotor for Me-groups'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.043P)^2^+0.420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                7497
_reflns_number_total             8052
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029048ysi20021022_034217_1.cif
_cod_data_source_block           (1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct method' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1780.9(2)
_cod_database_code               4113775