Tetrachlorobis(<i>N</i>^1^-phenylacetamidino-κ<i>N</i>^2^)rhenium(IV) at 11K by X-ray diffraction and at 20K by neutron diffraction
Figgis, Brian N.; Sobolev, Alexandre N.; Schultz, Arthur J.; Reynolds, Philip A.; Acta Crystallographica Section C 57 (2001) 1151–1153; doi:10.1107/S0108270101011659

data_2012252
_publ_section_title
;
 Tetrachlorobis(<i>N</i>^1^-phenylacetamidino-\k<i>N</i>^2^)rhenium(IV)
 at 11K by X-ray diffraction and at 20K by neutron diffraction
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1151
_journal_page_last               1153
_journal_paper_doi               10.1107/S0108270101011659
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Re Cl4 (C8 H10 N2)2]'
_chemical_formula_moiety         'C16 H20 Cl4 N4 Re'
_chemical_formula_sum            'C16 H20 Cl4 N4 Re'
_chemical_formula_weight         596.36
_chemical_name_common            bis(N-phenylacetamidino)ReCl~4~
_chemical_name_systematic
;
Tetrachlorobis(N^1^-phenylacetamidino-N^2^)rhenium(IV)
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.604(4)
_cell_length_b                   7.2680(10)
_cell_length_c                   12.436(2)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    11(2)
_cell_measurement_theta_max      17.9
_cell_measurement_theta_min      15.3
_cell_volume                     1952.7(5)
_computing_cell_refinement       'local diffractometer control software'
_computing_data_collection       'local diffractometer control software'
_computing_data_reduction        'PROFIT (Streltsov & Zavodnik, 1989)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      11(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Huber 512 goniometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .026
_diffrn_reflns_av_sigmaI/netI    .029
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5671
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.778
_exptl_absorpt_correction_T_max  .297
_exptl_absorpt_correction_T_min  .238
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(Xtal3.7; Hall et al., 2000)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bipyramid
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          .26
_exptl_crystal_size_mid          .26
_exptl_crystal_size_min          .25
_refine_diff_density_max         1.58
_refine_diff_density_min         -2.01
_refine_ls_extinction_coef       .00123(10)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          .029
_refine_ls_R_factor_gt           .022
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0228P)^2^+1.5368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .051
_reflns_number_gt                2406
_reflns_number_total             2873
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd1153.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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 'Gaussian'
changed to 'gaussian' 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_sg_symbol_H-M      Pccn
_cod_database_code               2012252
_cod_database_fobs_code          2012252