Syntheses and characterisation of methyltrioxorhenium adducts of low-valence organometallic Lewis bases
Santos, Ana M.; Kühn, Fritz E.; Xue, Wen-Mei; Herdtweck, Eberhardt; Journal of the Chemical Society, Dalton Transactions  (2000) 3570–; doi:10.1039/b004640j

data_7009951
_publ_section_title
;
 Syntheses and characterisation of methyltrioxorhenium adducts of
 low-valence organometallic Lewis bases
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3570
_journal_paper_doi               10.1039/b004640j
_journal_year                    2000
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C18 H16 Fe N O3 Re'
_chemical_formula_sum            'C18 H16 Fe N O3 Re'
_chemical_formula_weight         536.38
_chemical_name_systematic
;
 (4-Ferrocenylethynylpyridine)methyltrioxorhenium
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                68.94(2)
_cell_angle_beta                 77.44(2)
_cell_angle_gamma                75.59(1)
_cell_formula_units_Z            2
_cell_length_a                   5.9809(6)
_cell_length_b                   11.495(2)
_cell_length_c                   13.719(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.8
_cell_measurement_theta_min      8.6
_cell_volume                     843.9(2)
_computing_cell_refinement       'IPDS (STOE)'
_computing_data_collection       'IPDS (STOE)'
_computing_data_reduction        'IPDS (STOE)'
_computing_molecular_graphics    'PLATON (Spek, 1999)'
_computing_publication_material  'PLATON (Spek, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1992)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device       'IPDS (STOE)'
_diffrn_measurement_method       ' oscillation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11532
_diffrn_reflns_theta_full        25.56
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.040
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 using DIFABS strategy
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    2.111
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.247
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.247
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+4.4621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0663
_reflns_number_gt                2654
_reflns_number_total             2945
_reflns_observed_criterion       >2sigma(i)
_cod_data_source_file            b004640j.txt
_cod_data_source_block           ANAC-3086-173
_cod_depositor_comments
;
 Updating the _chemical_name_systematic data item value after consulting
 the original publication.

 Antanas Vaitkus,
 2017-03-29

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value ' empirical ' changed
to 'empirical' 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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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^)+(0.0153P)^2^+4.4621P] 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^)+(0.0153P)^2^+4.4621P] 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               7009951