Mixed-Ligand Complexes of Technetium. XIV. Structure of <i>trans</i>-[TcCl~2~(NCS)(Me~2~PhP)~3~]
Abram, U.; Abram, S.; Dilworth, J. R.; Acta Crystallographica Section C 52 (1996) 605–607; doi:10.1107/S0108270195012923

data_2004621
_publ_section_title
;
 Mixed-Ligand Complexes of Technetium. XIV. Structure of
 <i>trans</i>-[TcCl~2~(NCS)(Me~2~PhP)~3~]
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              605
_journal_page_last               607
_journal_paper_doi               10.1107/S0108270195012923
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Tc Cl2 (N C S) (C8 H11 P)3)]'
_chemical_formula_moiety         '[TcCl~2~(Me~2~PhP)~3~(NCS)]'
_chemical_formula_sum            'C25 H33 Cl2 N P3 S Tc'
_chemical_formula_weight         '641.39 (based on ~99~Tc)'
_chemical_name_systematic
;
 trans-Dichlorotris(dimethylphenylphosphine)isothiocyanatotechnetium(III)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 113.04(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.997(7)
_cell_length_b                   10.840(2)
_cell_length_c                   19.160(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      13.58
_cell_measurement_theta_min      7.79
_cell_volume                     2866.3(19)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'CAD-4 Software, SDP (Frenz, 1983), HKL (Kretschmar, 1994)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1994)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'CAD4 ENRAF NONIUS'
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0858
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8402
_diffrn_reflns_theta_max         28.93
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        insignificant
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.9998
_exptl_absorpt_correction_T_min  0.9764
_exptl_absorpt_correction_type   '\y scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.658
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.155
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_hydrogen_treatment    'H atoms refined freely'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_obs          0.0491
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0044P)^2^+3.1020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0891
_refine_ls_wR_factor_obs         0.0668
_reflns_number_observed          4918
_reflns_number_total             7582
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            jz1079.cif
_cod_data_source_block           ncs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (17 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0044P)^2^+3.1020P] 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^)+(0.0044P)^2^+3.1020P] 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        2866(2)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               2004621