Tricarbonyl[1,1',1''-ethylidynetris(pyrazole-κ<i>N</i>^2^)]rhenium(I) bromide and tricarbonyl[methylidynetris(pyrazole-κ<i>N</i>^2^)]rhenium(I) iodide ethanol hemisolvate
Gibson, Dorothy H.; Mashuta, Mark S.; He, Haiyang; Acta Crystallographica Section C 57 (2001) 1135–1137; doi:10.1107/S0108270101009349

data_2012242
_publ_section_title
;
 Tricarbonyl[1,1',1''-ethylidynetris(pyrazole-\k<i>N</i>^2^)]rhenium(I)
 bromide and
 tricarbonyl[methylidynetris(pyrazole-\k<i>N</i>^2^)]rhenium(I) iodide
 ethanol hemisolvate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1135
_journal_page_last               1137
_journal_paper_doi               10.1107/S0108270101009349
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Re (C11 H12 N6 )(C O)3] I, 0.5C2 H6 O'
_chemical_formula_moiety         'C14 H12 N6 O3 Re 1+, I 1-, 0.5C2 H6 O'
_chemical_formula_sum            'C15 H15 I N6 O3.5 Re'
_chemical_formula_weight         648.44
_chemical_name_common
; tricarbonyl-methyltris(pyrazol-1-yl)methane rhenium(I)
  iodide ethanol hemisolvate
;
_chemical_name_systematic
; tricarbonyl-methyltris(pyrazol-1-yl)methane rhenium(I)
  iodide ethanol solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.83(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.361(3)
_cell_length_b                   11.803(2)
_cell_length_c                   15.543(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      15.0
_cell_volume                     2146.3(8)
_computing_cell_refinement       'CAD-4 Diffractometer Control Software'
_computing_data_collection
'CAD-4 Diffractometer Control Software (Enraf-Nonius, 1988)'
_computing_data_reduction        'SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  'equatorial mounted graphite'
_diffrn_radiation_source         'normal focus Philips sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .068
_diffrn_reflns_av_sigmaI/netI    .0215
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5073
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.13
_exptl_absorpt_correction_T_max  .20
_exptl_absorpt_correction_T_min  .08
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details
;
 North et al. (1968)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.022
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1233
_exptl_crystal_size_max          .41
_exptl_crystal_size_mid          .23
_exptl_crystal_size_min          .23
_refine_diff_density_max         1.37
_refine_diff_density_min         -1.29
_refine_ls_extinction_coef       .0094(5)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          .056
_refine_ls_R_factor_gt           .045
_refine_ls_shift/su_max          .014
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0778P)^2^+1.9504P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .123
_reflns_number_gt                4128
_reflns_number_total             4896
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bk1610.cif
_cod_data_source_block           II
_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_enum 1527 2010-12-29 10:47:43Z saulius 

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 
;
_cod_original_cell_volume        2146.3(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C15 H15 I N6 O3.50 Re'
_cod_database_code               2012242