#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:08:33 +0100 (lun 21 de mar de 2016) $
#$Revision: 178596 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/07/4070769.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4070769
loop_
_publ_author_name
'Han, Ying-Feng'
'Huang, Yuan-Biao'
'Lin, Yue-Jian'
'Jin, Guo-Xin'
_publ_section_title
;
 Synthesis, Characterization, and Norbornene Polymerization Behavior of
 the Half-Sandwich Complexes [Cp*3M3(μ3-L)Cl3] and [Cp*M(2-SPyH)Cl2] (M =
 Ir, M = Rh, [L]3−= 1,3,5-Triazine-2,4,6-trithiolato, 2-SPy =
 2-Pyridinethione)
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              961
_journal_paper_doi               10.1021/om7010003
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C15 H20 Cl2 Ir N S'
_chemical_formula_weight         509.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   9.11(4)
_cell_length_b                   16.00(7)
_cell_length_c                   23.70(10)
_cell_measurement_reflns_used    963
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.894
_cell_measurement_theta_min      2.692
_cell_volume                     3455(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      293(2)
_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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15911
_diffrn_reflns_theta_full        27.24
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        11.79
_exptl_absorpt_coefficient_mu    8.151
_exptl_absorpt_correction_T_max  0.4961
_exptl_absorpt_correction_T_min  0.2351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.573
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3834
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0347P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                2808
_reflns_number_total             3834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7010003-file003.cif
_cod_data_source_block           f61227c
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3454(25)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4070769
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ir1 Ir 0.95642(2) 0.645271(11) 0.613039(8) 0.03346(8) Uani 1 1 d .
S1 S 0.98749(16) 0.49977(8) 0.62307(6) 0.0459(3) Uani 1 1 d .
Cl1 Cl 1.00235(17) 0.67072(8) 0.71290(6) 0.0471(3) Uani 1 1 d .
Cl2 Cl 1.21671(15) 0.66705(10) 0.59737(7) 0.0565(4) Uani 1 1 d .
N1 N 1.2207(5) 0.5209(3) 0.69045(19) 0.0475(11) Uani 1 1 d D
C1 C 1.1390(6) 0.4684(3) 0.6599(2) 0.0378(11) Uani 1 1 d .
C2 C 1.1813(6) 0.3848(3) 0.6607(2) 0.0477(13) Uani 1 1 d .
H2 H 1.1286 0.3456 0.6400 0.057 Uiso 1 1 calc R
C3 C 1.2996(7) 0.3600(4) 0.6918(2) 0.0584(16) Uani 1 1 d .
H3 H 1.3270 0.3040 0.6920 0.070 Uiso 1 1 calc R
C4 C 1.3792(7) 0.4170(4) 0.7228(3) 0.0618(17) Uani 1 1 d .
H4 H 1.4596 0.3999 0.7441 0.074 Uiso 1 1 calc R
C5 C 1.3388(7) 0.4969(4) 0.7217(3) 0.0590(16) Uani 1 1 d .
H5 H 1.3912 0.5364 0.7423 0.071 Uiso 1 1 calc R
C6 C 0.7247(5) 0.6498(4) 0.5988(2) 0.0514(14) Uani 1 1 d .
C7 C 0.7726(6) 0.7306(4) 0.6120(2) 0.0540(15) Uani 1 1 d .
C8 C 0.8786(6) 0.7567(3) 0.5713(2) 0.0460(13) Uani 1 1 d .
C9 C 0.8936(6) 0.6897(3) 0.5310(2) 0.0425(12) Uani 1 1 d .
C10 C 0.7976(6) 0.6242(3) 0.5474(2) 0.0451(13) Uani 1 1 d .
C11 C 0.6096(7) 0.5965(5) 0.6288(3) 0.087(2) Uani 1 1 d .
H11A H 0.5684 0.6276 0.6596 0.130 Uiso 1 1 calc R
H11B H 0.6548 0.5465 0.6429 0.130 Uiso 1 1 calc R
H11C H 0.5332 0.5819 0.6026 0.130 Uiso 1 1 calc R
C12 C 0.7211(8) 0.7835(5) 0.6608(3) 0.090(3) Uani 1 1 d .
H12A H 0.6255 0.8056 0.6526 0.135 Uiso 1 1 calc R
H12B H 0.7887 0.8288 0.6666 0.135 Uiso 1 1 calc R
H12C H 0.7164 0.7499 0.6943 0.135 Uiso 1 1 calc R
C13 C 0.9549(8) 0.8384(4) 0.5661(4) 0.077(2) Uani 1 1 d .
H13A H 0.9485 0.8681 0.6012 0.115 Uiso 1 1 calc R
H13B H 0.9093 0.8708 0.5368 0.115 Uiso 1 1 calc R
H13C H 1.0562 0.8292 0.5568 0.115 Uiso 1 1 calc R
C14 C 0.9890(7) 0.6929(4) 0.4798(2) 0.0585(16) Uani 1 1 d .
H14A H 0.9985 0.6377 0.4643 0.088 Uiso 1 1 calc R
H14B H 1.0842 0.7137 0.4900 0.088 Uiso 1 1 calc R
H14C H 0.9455 0.7293 0.4523 0.088 Uiso 1 1 calc R
C15 C 0.7704(7) 0.5444(4) 0.5157(3) 0.0644(17) Uani 1 1 d .
H15A H 0.6808 0.5491 0.4947 0.097 Uiso 1 1 calc R
H15B H 0.7627 0.4989 0.5420 0.097 Uiso 1 1 calc R
H15C H 0.8505 0.5342 0.4903 0.097 Uiso 1 1 calc R
H1 H 1.188(6) 0.5701(17) 0.694(2) 0.049(16) Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C6 Ir1 C9 65.4(2)
C6 Ir1 C10 39.4(2)
C9 Ir1 C10 38.6(2)
C6 Ir1 C8 64.9(2)
C9 Ir1 C8 39.16(19)
C10 Ir1 C8 65.0(3)
C6 Ir1 C7 38.0(3)
C9 Ir1 C7 64.8(2)
C10 Ir1 C7 64.5(3)
C8 Ir1 C7 38.6(2)
C6 Ir1 S1 99.68(17)
C9 Ir1 S1 116.74(16)
C10 Ir1 S1 89.94(17)
C8 Ir1 S1 154.35(17)
C7 Ir1 S1 135.9(2)
C6 Ir1 Cl2 159.36(19)
C9 Ir1 Cl2 94.3(2)
C10 Ir1 Cl2 124.7(3)
C8 Ir1 Cl2 97.6(2)
C7 Ir1 Cl2 131.7(3)
S1 Ir1 Cl2 92.29(10)
C6 Ir1 Cl1 108.48(16)
C9 Ir1 Cl1 150.4(2)
C10 Ir1 Cl1 147.52(18)
C8 Ir1 Cl1 111.3(2)
C7 Ir1 Cl1 92.22(17)
S1 Ir1 Cl1 92.66(10)
Cl2 Ir1 Cl1 87.53(12)
C1 S1 Ir1 116.04(18)
C1 N1 C5 123.9(5)
N1 C1 C2 116.3(5)
N1 C1 S1 122.8(4)
C2 C1 S1 120.8(4)
C3 C2 C1 120.3(5)
C2 C3 C4 120.8(6)
C5 C4 C3 118.6(6)
C4 C5 N1 120.0(5)
C7 C6 C10 107.9(5)
C7 C6 C11 128.8(6)
C10 C6 C11 123.3(6)
C7 C6 Ir1 71.8(3)
C10 C6 Ir1 70.7(3)
C11 C6 Ir1 125.8(4)
C6 C7 C8 109.3(5)
C6 C7 C12 126.4(6)
C8 C7 C12 124.3(6)
C6 C7 Ir1 70.2(4)
C8 C7 Ir1 70.6(4)
C12 C7 Ir1 125.9(4)
C7 C8 C9 107.1(5)
C7 C8 C13 129.1(6)
C9 C8 C13 123.6(6)
C7 C8 Ir1 70.8(3)
C9 C8 Ir1 70.0(4)
C13 C8 Ir1 127.7(5)
C10 C9 C8 107.9(5)
C10 C9 C14 127.4(5)
C8 C9 C14 124.6(5)
C10 C9 Ir1 70.8(3)
C8 C9 Ir1 70.8(4)
C14 C9 Ir1 126.3(4)
C9 C10 C6 107.7(5)
C9 C10 C15 126.3(5)
C6 C10 C15 125.9(5)
C9 C10 Ir1 70.6(3)
C6 C10 Ir1 69.9(4)
C15 C10 Ir1 127.3(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ir1 C6 2.139(10)
Ir1 C9 2.147(9)
Ir1 C10 2.151(8)
Ir1 C8 2.158(8)
Ir1 C7 2.160(8)
Ir1 S1 2.357(9)
Ir1 Cl2 2.425(10)
Ir1 Cl1 2.438(10)
S1 C1 1.709(7)
N1 C1 1.335(7)
N1 C5 1.361(8)
C1 C2 1.392(8)
C2 C3 1.364(9)
C3 C4 1.377(9)
C4 C5 1.332(9)
C6 C7 1.399(9)
C6 C10 1.446(9)
C6 C11 1.527(9)
C7 C8 1.426(8)
C7 C12 1.509(9)
C8 C9 1.443(8)
C8 C13 1.486(9)
C9 C10 1.419(8)
C9 C14 1.492(9)
C10 C15 1.501(9)
