N-Metallation of MS2N2 rings. X-ray crystal structures of [(?5-C5Me5)Ir(S2N2)Au(PPh3)][ClO4], [{(?5-C5Me5)Ir(S2N2)Au}2(�2-dppm)][ClO4]2 and [Au(dppeS-P)Cl]2
Aucott, Stephen M.; Bhattacharyya, Pravat; Milton, Heather L.; Slawin, Alexandra M. Z.; Woollins, J. Derek; New Journal of Chemistry 27 (2003) 1466–; doi:10.1039/b306847a

data_7050651
_publ_section_title
;
 N-Metallation of MS2N2 rings. X-ray crystal structures of
 [(?5-C5Me5)Ir(S2N2)Au(PPh3)][ClO4],
 [{(?5-C5Me5)Ir(S2N2)Au}2(&#xFFFD;2-dppm)][ClO4]2 and [Au(dppeS-P)Cl]2
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1466
_journal_paper_doi               10.1039/b306847a
_journal_volume                  27
_journal_year                    2003
_chemical_formula_moiety         'C28 H30 Au Cl Ir N2 O4 P S2'
_chemical_formula_sum            'C28 H30 Au Cl Ir N2 O4 P S2'
_chemical_formula_weight         978.25
_chemical_melting_point          ?
_chemical_name_systematic        '[(h5-C5Me5)Ir(S2N2)Au(PPh3)][ClO4]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.213(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0057(17)
_cell_length_b                   11.2301(15)
_cell_length_c                   21.098(3)
_cell_measurement_reflns_used    159
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     3049.9(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_detector_area_resol_mean 0.9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14834
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    9.477
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.631559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   -
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.130
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.00027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         4361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0479
_reflns_number_gt                3616
_reflns_number_total             4361
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306847a.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'MULTISCAN' changed to
'multi-scan' according to
'/home/adriana/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 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '-' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' 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      P2(1)/c
_cod_database_code               7050651