Synthesis, Crystal Structure, High-Resolution Optical Spectroscopy, and Extended Hückel Calculations for [Re(CO)4(thpy)] (thpy-= 2-(2-Thienyl)pyridinate). Comparison with Related Cyclometalated Complexes
Frederik W. M. Vanhelmont; Hans U. Güdel; Inorganic Chemistry 36 (1997) 5512–5517; doi:10.1021/ic970415u

data_4323673
_publ_section_title
;
 Synthesis, Crystal Structure, High-Resolution Optical Spectroscopy, and
 Extended H\"uckel Calculations for [Re(CO)4(thpy)] (thpy-=
 2-(2-Thienyl)pyridinate). Comparison with Related Cyclometalated
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5512
_journal_page_last               5517
_journal_paper_doi               10.1021/ic970415u
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source
;
Give summary of chemical and crystal preparation
in sufficent detail to reproduce experiment
;
_chemical_formula_moiety         'C4 O4 Re 1+, C9 H6 N S 1-'
_chemical_formula_sum            'C13 H6 N O4 Re S'
_chemical_formula_weight         458.45
_chemical_name_systematic
; 
2-(2-thienyl)pyridine)-tetracarbonyl-rhenium(I)
;
_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                 110.33(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.64(7)
_cell_length_b                   11.70(13)
_cell_length_c                   12.23(6)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.97
_cell_measurement_theta_min      2.04
_cell_volume                     1428(2)
_computing_cell_refinement       'CAD4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'SHELXTL PC^TM^ (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4265
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.664
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.6991
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.952
_refine_ls_extinction_coef       0.0067(2)
_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_all   1.023
_refine_ls_goodness_of_fit_obs   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_restrained_S_obs      1.062
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_obs          0.0260
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+1.7346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0611
_refine_ls_wR_factor_obs         0.0534
_reflns_number_observed          2489
_reflns_number_total             3429
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970415u.cif
_cod_data_source_block           rhen.acta
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+1.7346P] 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^)+(0.0225P)^2^+1.7346P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1430(20)
_cod_database_code               4323673