Tertiary phosphine binding to pyridylazole chelated rhenium via substitution in phosphine oxide precursors: geometrical preference, twin isomerization and effects of diphosphine spacer length and metal oxidation state
Sengupta, Suman; Gangopadhyay, Jaydip; Chakravorty, Animesh; Dalton Transactions  (2003) 4635–; doi:10.1039/b307834e

data_7013434
_publ_section_title
;
 Tertiary phosphine binding to pyridylazole chelated rhenium via
 substitution in phosphine oxide precursors: geometrical preference,
 twin isomerization and effects of diphosphine spacer length and metal
 oxidation state
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4635
_journal_paper_doi               10.1039/b307834e
_journal_year                    2003
_chemical_formula_sum            'C30.5 H24 Cl4 N3 O4 P Re S'
_chemical_formula_weight         887.56
_chemical_name_systematic
;
?
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                86.26(3)
_cell_angle_beta                 88.95(3)
_cell_angle_gamma                75.15(3)
_cell_formula_units_Z            4
_cell_length_a                   13.989(3)
_cell_length_b                   14.769(3)
_cell_length_c                   16.881(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7
_cell_volume                     3364.0(13)
_computing_cell_refinement       'Siemens P3/P4-PC V4.27'
_computing_data_collection       'Siemens P3/P4-PC V4.27'
_computing_data_reduction        'Siemens P3/P4-PC V4.27'
_computing_molecular_graphics    'Siemens SHELXTL V5.03 PC'
_computing_publication_material  'Siemens SHELXTL V5.03 PC'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       '\w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10539
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.079
_exptl_absorpt_correction_T_max  0.215
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_description       Parallopiped
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.684
_refine_diff_density_min         -3.227
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.085
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         10501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_restrained_S_obs      1.085
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_obs          0.0595
_refine_ls_shift/esd_max         -0.343
_refine_ls_shift/esd_mean        0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1078P)^2^+7.1029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1710
_refine_ls_wR_factor_obs         0.1482
_reflns_number_observed          8711
_reflns_number_total             10539
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b307834e.txt
_cod_data_source_block           test7
_cod_depositor_comments
;
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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1078P)^2^+7.1029P] 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^)+(0.1078P)^2^+7.1029P] where P=(Fo^2^+2Fc^2^)/3'.

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

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Heavy atom method' was changed
to 'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3364.1(12)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C30.50 H24 Cl4 N3 O4 P Re S'
_cod_database_code               7013434