New Cyanometalate Building Units: Synthesis and Characterization of [Re(CN)7]3- and [Re(CN)8]3-
Miriam V. Bennett; Jeffrey R. Long; Journal of the American Chemical Society 125 (2003) 2394–2395; doi:10.1021/ja029795v

data_4113524
_publ_contact_author
;
        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_email       jlong@cchem.berkeley.edu
_publ_contact_author_fax         '510 643-3832'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 New Cyanometalate Building Units: Synthesis and Characterization of
 [Re(CN)7]3- and [Re(CN)8]3-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2394
_journal_page_last               2395
_journal_paper_doi               10.1021/ja029795v
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source        synthetic
_chemical_formula_structural     K3Re(CN)3-2MeCN
_chemical_formula_sum            'C12 H6 K3 N10 Re'
_chemical_formula_weight         593.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2149(5)
_cell_length_b                   10.5170(3)
_cell_length_c                   9.3391(3)
_cell_measurement_temperature    134(2)
_cell_volume                     1690.84(9)
_computing_cell_refinement
;
  SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
  SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      134(2)
_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  0.0502
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7163
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    7.946
_exptl_absorpt_correction_type   'gaussian from xtal shape'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.333
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.911
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.005
_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_obs          0.0194
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0440
_refine_ls_wR_factor_obs         0.0438
_reflns_number_observed          1391
_reflns_number_total             1570
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja029795v_s2_3.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+0.0000P] 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^)+(0.0173P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4113524