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_7050652
_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
'C44 H53 Au2 Ir2 N4 P2 S4.[Cl O4]2.[C2 H2 Cl2]'
_chemical_formula_sum            'C46 H55 Au2 Cl4 Ir2 N4 O8 P2 S4'
_chemical_formula_weight         1902.25
_chemical_melting_point          ?
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.363(8)
_cell_length_b                   10.367(3)
_cell_length_c                   16.838(4)
_cell_measurement_reflns_used    307
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     5649(3)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23332
_diffrn_reflns_theta_full        23.33
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    10.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.702289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   -
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.237
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3588
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       -
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         7349
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+5.5123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                7056
_reflns_number_total             7349
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306847a.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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      Pca2(1)
_cod_database_code               7050652