#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/10/7001017.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_7001017
loop_
_publ_author_name
'Kimura, Takashi'
'Arita, Hiroko'
'Ishiwata, Koji'
'Kuwata, Shigeki'
'Ikariya, Takao'
_publ_section_title
;
 Synthesis of parent amido (NH2)-bridged dinuclear complexes of
 ruthenium and iridium by stepwise transfer hydrogenation of μ-azido
 complexes
;
_journal_issue                   16
_journal_name_full               'Dalton Transactions'
_journal_page_first              2912
_journal_page_last               2914
_journal_paper_doi               10.1039/b902810m
_journal_year                    2009
_chemical_formula_moiety         'C20 H33 Cl2 Ir2 N '
_chemical_formula_sum            'C20 H33 Cl2 Ir2 N'
_chemical_formula_weight         742.83
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.449(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   19.250(9)
_cell_length_b                   13.076(6)
_cell_length_c                   9.060(4)
_cell_measurement_reflns_used    3829
_cell_measurement_temperature    293.1
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      3.0
_cell_volume                     2278.4(18)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR2002
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9859
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         31.33
_exptl_absorpt_coefficient_mu    11.939
_exptl_absorpt_correction_T_max  0.303
_exptl_absorpt_correction_T_min  0.070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.04
_refine_diff_density_min         -1.10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2528
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0009Fo² + 0.5000σ(Fo²)]/(4Fo²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                1991
_reflns_number_total             2529
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            b902810m.txt
_cod_data_source_block           '__2b'
_cod_original_cell_volume        2278.6(19)
_cod_original_formula_sum        'C20 H33 Cl2 Ir2 N '
_cod_database_code               7001017
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-Y,1/2+Z
5 1/2+X,1/2+Y,+Z
6 1/2-X,1/2+Y,1/2-Z
7 1/2-X,1/2-Y,-Z
8 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir(1) Ir 0.426600(10) 0.28135(2) 0.71961(2) 0.03215(8) Uani 1.00 1 d . . .
Cl(1) Cl 0.40876(12) 0.3088(2) 0.9782(2) 0.0646(6) Uani 1.00 1 d . . .
N(1) N 0.500000(10) 0.3958(6) 0.750000(10) 0.040(2) Uani 1.00 2 d S . .
C(1) C 0.3624(3) 0.1602(6) 0.6220(8) 0.0464(19) Uani 1.00 1 d . . .
C(2) C 0.3183(4) 0.2348(9) 0.6778(9) 0.060(2) Uani 1.00 1 d . . .
C(3) C 0.3322(4) 0.3318(7) 0.6015(9) 0.053(2) Uani 1.00 1 d . . .
C(4) C 0.3849(4) 0.3107(6) 0.4985(7) 0.0454(19) Uani 1.00 1 d . . .
C(5) C 0.4027(4) 0.2050(5) 0.5111(7) 0.0411(18) Uani 1.00 1 d . . .
C(6) C 0.3631(7) 0.0472(8) 0.6659(14) 0.107(4) Uani 1.00 1 d . . .
C(7) C 0.2652(6) 0.2240(14) 0.7900(13) 0.119(5) Uani 1.00 1 d . . .
C(8) C 0.2958(5) 0.4305(10) 0.6235(14) 0.105(4) Uani 1.00 1 d . . .
C(9) C 0.4144(5) 0.3831(7) 0.3907(10) 0.067(2) Uani 1.00 1 d . . .
C(10) C 0.4508(5) 0.1502(8) 0.4190(11) 0.078(3) Uani 1.00 1 d . . .
H(1) H 0.4939 0.4377 0.8341 0.047 Uiso 1.00 1 c R . .
H(2) H 0.5000 0.212(7) 0.7500 0.04(3) Uiso 1.00 2 d S . .
H(3) H 0.3309 0.0361 0.7408 0.126 Uiso 1.00 1 c R . .
H(4) H 0.3507 0.0059 0.5825 0.126 Uiso 1.00 1 c R . .
H(5) H 0.4086 0.0296 0.7023 0.126 Uiso 1.00 1 c R . .
H(6) H 0.2422 0.2873 0.8040 0.143 Uiso 1.00 1 c R . .
H(7) H 0.2323 0.1737 0.7584 0.143 Uiso 1.00 1 c R . .
H(8) H 0.2881 0.2034 0.8801 0.143 Uiso 1.00 1 c R . .
H(9) H 0.3134 0.4796 0.5575 0.124 Uiso 1.00 1 c R . .
H(10) H 0.2473 0.4213 0.6035 0.124 Uiso 1.00 1 c R . .
H(11) H 0.3034 0.4536 0.7223 0.124 Uiso 1.00 1 c R . .
H(12) H 0.4474 0.3489 0.3332 0.080 Uiso 1.00 1 c R . .
H(13) H 0.3777 0.4086 0.3276 0.080 Uiso 1.00 1 c R . .
H(14) H 0.4363 0.4385 0.4419 0.080 Uiso 1.00 1 c R . .
H(15) H 0.4525 0.0803 0.4474 0.094 Uiso 1.00 1 c R . .
H(16) H 0.4353 0.1550 0.3183 0.094 Uiso 1.00 1 c R . .
H(17) H 0.4958 0.1795 0.4324 0.094 Uiso 1.00 1 c R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
Cl Cl 0.148 0.159
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ir Ir -1.444 7.990
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, 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
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
Ir(1) Ir(1) Cl(1) 89.63(5) yes 2_656 . .
Ir(1) Ir(1) N(1) 46.34(15) yes 2_656 . .
Ir(1) Ir(1) C(1) 128.3(2) yes 2_656 . .
Ir(1) Ir(1) C(2) 163.8(3) yes 2_656 . .
Ir(1) Ir(1) C(3) 153.5(2) yes 2_656 . .
Ir(1) Ir(1) C(4) 120.3(2) yes 2_656 . .
Ir(1) Ir(1) C(5) 109.8(2) yes 2_656 . .
Cl(1) Ir(1) N(1) 83.55(6) yes . . .
Cl(1) Ir(1) C(1) 113.7(2) yes . . .
Cl(1) Ir(1) C(2) 92.0(2) yes . . .
Cl(1) Ir(1) C(3) 106.4(2) yes . . .
Cl(1) Ir(1) C(4) 144.4(2) yes . . .
Cl(1) Ir(1) C(5) 151.9(2) yes . . .
N(1) Ir(1) C(1) 162.7(2) yes . . .
N(1) Ir(1) C(2) 149.8(3) yes . . .
N(1) Ir(1) C(3) 113.5(2) yes . . .
N(1) Ir(1) C(4) 102.7(2) yes . . .
N(1) Ir(1) C(5) 124.6(2) yes . . .
C(1) Ir(1) C(2) 37.5(3) yes . . .
C(1) Ir(1) C(3) 64.6(3) yes . . .
C(1) Ir(1) C(4) 64.5(2) yes . . .
C(1) Ir(1) C(5) 38.2(2) yes . . .
C(2) Ir(1) C(3) 39.5(3) yes . . .
C(2) Ir(1) C(4) 64.9(3) yes . . .
C(2) Ir(1) C(5) 63.7(3) yes . . .
C(3) Ir(1) C(4) 38.7(3) yes . . .
C(3) Ir(1) C(5) 64.5(3) yes . . .
C(4) Ir(1) C(5) 38.5(2) yes . . .
Ir(1) N(1) Ir(1) 87.3(3) yes . . 2_656
Ir(1) C(1) C(2) 71.8(5) yes . . .
Ir(1) C(1) C(5) 70.7(4) yes . . .
Ir(1) C(1) C(6) 126.8(6) yes . . .
C(2) C(1) C(5) 109.0(7) yes . . .
C(2) C(1) C(6) 125.3(8) yes . . .
C(5) C(1) C(6) 125.6(7) yes . . .
Ir(1) C(2) C(1) 70.7(4) yes . . .
Ir(1) C(2) C(3) 69.7(4) yes . . .
Ir(1) C(2) C(7) 126.1(6) yes . . .
C(1) C(2) C(3) 107.8(7) yes . . .
C(1) C(2) C(7) 128.9(11) yes . . .
C(3) C(2) C(7) 123.3(10) yes . . .
Ir(1) C(3) C(2) 70.8(4) yes . . .
Ir(1) C(3) C(4) 70.2(4) yes . . .
Ir(1) C(3) C(8) 126.0(6) yes . . .
C(2) C(3) C(4) 106.6(7) yes . . .
C(2) C(3) C(8) 126.0(8) yes . . .
C(4) C(3) C(8) 127.3(8) yes . . .
Ir(1) C(4) C(3) 71.1(4) yes . . .
Ir(1) C(4) C(5) 71.1(4) yes . . .
Ir(1) C(4) C(9) 125.8(5) yes . . .
C(3) C(4) C(5) 108.0(6) yes . . .
C(3) C(4) C(9) 127.1(7) yes . . .
C(5) C(4) C(9) 124.8(7) yes . . .
Ir(1) C(5) C(1) 71.1(4) yes . . .
Ir(1) C(5) C(4) 70.4(3) yes . . .
Ir(1) C(5) C(10) 127.4(6) yes . . .
C(1) C(5) C(4) 108.6(6) yes . . .
C(1) C(5) C(10) 125.5(7) yes . . .
C(4) C(5) C(10) 125.8(7) yes . . .
Ir(1) Ir(1) H(2) 32(2) no 2_656 . .
Cl(1) Ir(1) H(2) 94.3(3) no . . .
N(1) Ir(1) H(2) 79(2) no . . .
C(1) Ir(1) H(2) 98(2) no . . .
C(2) Ir(1) H(2) 131(2) no . . .
C(3) Ir(1) H(2) 156.7(15) no . . .
C(4) Ir(1) H(2) 121.4(4) no . . .
C(5) Ir(1) H(2) 92.2(16) no . . .
Ir(1) N(1) H(1) 114.7 no . . .
Ir(1) N(1) H(1) 114.7 no . . 2_656
Ir(1) N(1) H(1) 114.7 no 2_656 . .
Ir(1) N(1) H(1) 114.7 no 2_656 . 2_656
H(1) N(1) H(1) 109.5 no . . 2_656
C(1) C(6) H(3) 109.5 no . . .
C(1) C(6) H(4) 110.0 no . . .
C(1) C(6) H(5) 108.8 no . . .
H(3) C(6) H(4) 109.4 no . . .
H(3) C(6) H(5) 109.5 no . . .
H(4) C(6) H(5) 109.6 no . . .
C(2) C(7) H(6) 110.4 no . . .
C(2) C(7) H(7) 109.4 no . . .
C(2) C(7) H(8) 108.1 no . . .
H(6) C(7) H(7) 109.5 no . . .
H(6) C(7) H(8) 109.5 no . . .
H(7) C(7) H(8) 110.0 no . . .
C(3) C(8) H(9) 108.6 no . . .
C(3) C(8) H(10) 109.1 no . . .
C(3) C(8) H(11) 110.3 no . . .
H(9) C(8) H(10) 110.0 no . . .
H(9) C(8) H(11) 109.5 no . . .
H(10) C(8) H(11) 109.3 no . . .
C(4) C(9) H(12) 110.0 no . . .
C(4) C(9) H(13) 108.9 no . . .
C(4) C(9) H(14) 109.8 no . . .
H(12) C(9) H(13) 109.5 no . . .
H(12) C(9) H(14) 109.5 no . . .
H(13) C(9) H(14) 109.2 no . . .
C(5) C(10) H(15) 109.5 no . . .
C(5) C(10) H(16) 109.6 no . . .
C(5) C(10) H(17) 109.0 no . . .
H(15) C(10) H(16) 109.3 no . . .
H(15) C(10) H(17) 109.5 no . . .
H(16) C(10) H(17) 110.0 no . . .
Ir(1) H(2) Ir(1) 115(5) no . . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ir(1) Ir(1) 2.856(1) yes . 2_656
Ir(1) Cl(1) 2.4097(19) yes . .
Ir(1) N(1) 2.069(6) yes . .
Ir(1) C(1) 2.175(7) yes . .
Ir(1) C(2) 2.189(8) yes . .
Ir(1) C(3) 2.173(7) yes . .
Ir(1) C(4) 2.160(6) yes . .
Ir(1) C(5) 2.169(7) yes . .
C(1) C(2) 1.402(13) yes . .
C(1) C(5) 1.422(10) yes . .
C(1) C(6) 1.530(13) yes . .
C(2) C(3) 1.475(14) yes . .
C(2) C(7) 1.478(15) yes . .
C(3) C(4) 1.435(11) yes . .
C(3) C(8) 1.486(15) yes . .
C(4) C(5) 1.427(11) yes . .
C(4) C(9) 1.490(12) yes . .
C(5) C(10) 1.460(13) yes . .
Ir(1) H(2) 1.69(5) no . .
N(1) H(1) 0.950 no . .
N(1) H(1) 0.950 no . 2_656
C(6) H(3) 0.950 no . .
C(6) H(4) 0.950 no . .
C(6) H(5) 0.950 no . .
C(7) H(6) 0.950 no . .
C(7) H(7) 0.950 no . .
C(7) H(8) 0.950 no . .
C(8) H(9) 0.950 no . .
C(8) H(10) 0.950 no . .
C(8) H(11) 0.950 no . .
C(9) H(12) 0.950 no . .
C(9) H(13) 0.950 no . .
C(9) H(14) 0.950 no . .
C(10) H(15) 0.950 no . .
C(10) H(16) 0.950 no . .
C(10) H(17) 0.950 no . .
