Unprecedented Reduction of 2,2′-Bipyrimidine in a One-Pot Synthesis of Neutral Rhenium(I)-Based Molecular Rectangles
Wu, Jing-Yun; Thanasekaran, P.; Cheng, Yi-Wei; Lee, Chung-Chou; Manimaran, B.; Rajendran, T.; Liao, Rong-Tang; Lee, Gene-Hsiang; Peng, Shie-Ming; Lu, Kuang-Lieh; Organometallics 27 (2008) 2141–; doi:10.1021/om700873x

data_4070615
_publ_section_title
;
 Unprecedented Reduction of 2,2&#x2032;-Bipyrimidine in a One-Pot
 Synthesis of Neutral Rhenium(I)-Based Molecular Rectangles
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2141
_journal_paper_doi               10.1021/om700873x
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C36 H32 N12 O12 Re4'
_chemical_formula_weight         1569.54
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.338(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4514(1)
_cell_length_b                   13.0932(2)
_cell_length_c                   17.4539(1)
_cell_measurement_reflns_used    7529
_cell_measurement_temperature    150(1)
_cell_volume                     2150.54(4)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measurement_device       'Siemens SMART CCD'
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13065
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    11.296
_exptl_absorpt_correction_T_max  0.4920
_exptl_absorpt_correction_T_min  0.3138
_exptl_absorpt_correction_type   ' empirical used sadabs'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_density_meas      ?
_exptl_crystal_description       C56H70N8O12
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_obs          0.0390
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+6.3250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0685
_refine_ls_wR_factor_obs         0.0640
_reflns_number_observed          3930
_reflns_number_total             4847
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om700873x-file001.cif
_cod_data_source_block           ic7105
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+6.3250P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+6.3250P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4070615