#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:37:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179757 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/53/7005334.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_7005334
loop_
_publ_author_name
'Adams, Christopher J.'
'Baber, R. Angharad'
'Connelly, Neil G.'
'Harding, Phimphaka'
'Hayward, Owen D.'
'Kandiah, Mathivathani'
'Orpen, A. Guy'
_publ_section_title
;
 Iodination of triazenide-bridged rhodium and iridium complexes:
 oxidative addition vs. one-electron oxidation.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1325
_journal_page_last               1333
_journal_paper_doi               10.1039/b700736a
_journal_year                    2007
_chemical_formula_sum            'C33 H29 I2 N3 O P Rh'
_chemical_formula_weight         871.27
_chemical_name_systematic
;
?
;
_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'
_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                 97.006(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.252(2)
_cell_length_b                   18.050(3)
_cell_length_c                   19.716(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3268.0(11)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0935
_diffrn_reflns_av_sigmaI/netI    0.1223
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21320
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.491
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.5
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.876
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0165P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                4285
_reflns_number_total             7520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b700736a.txt
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3268.1(12)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7005334
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Rh1 Rh 0.77800(5) 0.88581(2) 0.77098(2) 0.02158(11) Uani 1 1 d . . .
C1 C 0.8948(6) 0.9336(3) 0.7128(3) 0.0286(14) Uani 1 1 d . . .
O1 O 0.9662(4) 0.9640(2) 0.6808(2) 0.0382(11) Uani 1 1 d . . .
I1 I 1.03173(4) 0.82478(2) 0.82647(2) 0.03172(11) Uani 1 1 d . . .
I2 I 0.74866(4) 0.78004(2) 0.67505(2) 0.03410(11) Uani 1 1 d . . .
P1 P 0.55800(16) 0.94392(8) 0.72662(8) 0.0257(4) Uani 1 1 d . . .
N1 N 0.7866(5) 0.9484(2) 0.8581(2) 0.0271(11) Uani 1 1 d . . .
N2 N 0.7148(5) 0.9050(3) 0.8952(2) 0.0282(12) Uani 1 1 d . . .
N3 N 0.6749(5) 0.8483(3) 0.8536(2) 0.0275(11) Uani 1 1 d . . .
C11 C 0.8546(6) 1.0129(3) 0.8885(3) 0.0287(14) Uani 1 1 d . . .
C12 C 0.8349(8) 1.0354(4) 0.9541(3) 0.063(2) Uani 1 1 d . . .
H12A H 0.7774 1.0064 0.9808 0.076 Uiso 1 1 calc R . .
C13 C 0.8986(9) 1.0994(4) 0.9803(3) 0.067(2) Uani 1 1 d . . .
H13A H 0.8833 1.1142 1.0251 0.081 Uiso 1 1 calc R . .
C14 C 0.9841(6) 1.1433(3) 0.9441(3) 0.0346(16) Uani 1 1 d . . .
C15 C 0.9997(6) 1.1205(3) 0.8790(3) 0.0396(16) Uani 1 1 d . . .
H15A H 1.0561 1.1501 0.8522 0.047 Uiso 1 1 calc R . .
C16 C 0.9365(6) 1.0563(3) 0.8507(3) 0.0352(15) Uani 1 1 d . . .
H16A H 0.9498 1.0423 0.8055 0.042 Uiso 1 1 calc R . .
C17 C 1.0532(7) 1.2136(3) 0.9733(3) 0.0498(19) Uani 1 1 d . . .
H17A H 1.0795 1.2449 0.9361 0.075 Uiso 1 1 calc R . .
H17B H 1.1410 1.2015 1.0044 0.075 Uiso 1 1 calc R . .
H17C H 0.9842 1.2401 0.9985 0.075 Uiso 1 1 calc R . .
C18 C 0.5958(6) 0.7911(3) 0.8806(3) 0.0314(15) Uani 1 1 d . . .
C19 C 0.5056(6) 0.8051(4) 0.9310(3) 0.0429(17) Uani 1 1 d . . .
H19A H 0.4958 0.8539 0.9479 0.051 Uiso 1 1 calc R . .
C20 C 0.4301(7) 0.7464(4) 0.9562(3) 0.051(2) Uani 1 1 d . . .
H20A H 0.3705 0.7557 0.9913 0.061 Uiso 1 1 calc R . .
C21 C 0.4395(7) 0.6756(4) 0.9319(4) 0.0497(19) Uani 1 1 d . . .
C22 C 0.5287(7) 0.6630(4) 0.8814(4) 0.0504(19) Uani 1 1 d . . .
H22A H 0.5366 0.6143 0.8639 0.060 Uiso 1 1 calc R . .
C23 C 0.6075(6) 0.7207(3) 0.8558(3) 0.0376(16) Uani 1 1 d . . .
H23A H 0.6687 0.7111 0.8214 0.045 Uiso 1 1 calc R . .
C24 C 0.3566(8) 0.6131(4) 0.9590(4) 0.081(3) Uani 1 1 d . . .
H24A H 0.3734 0.6131 1.0090 0.121 Uiso 1 1 calc R . .
H24B H 0.3898 0.5659 0.9417 0.121 Uiso 1 1 calc R . .
H24C H 0.2524 0.6193 0.9440 0.121 Uiso 1 1 calc R . .
C25 C 0.4111(6) 0.8840(3) 0.6890(3) 0.0271(13) Uani 1 1 d . . .
C26 C 0.3865(6) 0.8151(3) 0.7171(3) 0.0318(15) Uani 1 1 d . . .
H26A H 0.4511 0.7972 0.7547 0.038 Uiso 1 1 calc R . .
C27 C 0.2687(6) 0.7724(4) 0.6907(3) 0.0377(16) Uani 1 1 d . . .
H27A H 0.2522 0.7255 0.7103 0.045 Uiso 1 1 calc R . .
C28 C 0.1751(7) 0.7980(4) 0.6357(3) 0.0452(18) Uani 1 1 d . . .
H28A H 0.0944 0.7686 0.6175 0.054 Uiso 1 1 calc R . .
C29 C 0.1984(6) 0.8660(4) 0.6072(3) 0.0442(18) Uani 1 1 d . . .
H29A H 0.1341 0.8829 0.5691 0.053 Uiso 1 1 calc R . .
C30 C 0.3152(6) 0.9099(4) 0.6337(3) 0.0353(16) Uani 1 1 d . . .
H30A H 0.3298 0.9571 0.6144 0.042 Uiso 1 1 calc R . .
C31 C 0.5824(6) 1.0085(3) 0.6585(3) 0.0268(14) Uani 1 1 d . . .
C32 C 0.6442(6) 0.9823(3) 0.6021(3) 0.0305(14) Uani 1 1 d . . .
H32A H 0.6746 0.9321 0.6012 0.037 Uiso 1 1 calc R . .
C33 C 0.6621(6) 1.0284(3) 0.5470(3) 0.0360(16) Uani 1 1 d . . .
H33A H 0.7059 1.0097 0.5093 0.043 Uiso 1 1 calc R . .
C34 C 0.6165(6) 1.1008(3) 0.5472(3) 0.0368(16) Uani 1 1 d . . .
H34A H 0.6294 1.1327 0.5101 0.044 Uiso 1 1 calc R . .
C35 C 0.5523(7) 1.1265(3) 0.6017(3) 0.0407(17) Uani 1 1 d . . .
H35A H 0.5187 1.1763 0.6016 0.049 Uiso 1 1 calc R . .
C36 C 0.5352(6) 1.0809(3) 0.6574(3) 0.0338(15) Uani 1 1 d . . .
H36A H 0.4908 1.0999 0.6948 0.041 Uiso 1 1 calc R . .
C37 C 0.4814(6) 0.9955(3) 0.7924(3) 0.0260(14) Uani 1 1 d . . .
C38 C 0.3609(6) 0.9676(3) 0.8209(3) 0.0305(14) Uani 1 1 d . . .
H38A H 0.3142 0.9237 0.8029 0.037 Uiso 1 1 calc R . .
C39 C 0.3102(6) 1.0035(4) 0.8745(3) 0.0405(17) Uani 1 1 d . . .
H39A H 0.2296 0.9835 0.8939 0.049 Uiso 1 1 calc R . .
C40 C 0.3743(7) 1.0682(4) 0.9008(3) 0.0427(17) Uani 1 1 d . . .
H40A H 0.3375 1.0928 0.9377 0.051 Uiso 1 1 calc R . .
C41 C 0.4931(6) 1.0968(3) 0.8727(3) 0.0360(16) Uani 1 1 d . . .
H41A H 0.5383 1.1411 0.8904 0.043 Uiso 1 1 calc R . .
C42 C 0.5455(6) 1.0607(3) 0.8192(3) 0.0313(15) Uani 1 1 d . . .
H42A H 0.6266 1.0807 0.8002 0.038 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
P P 0.1023 0.0942 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 N1 107.0(2) . . ?
C1 Rh1 N3 166.5(2) . . ?
N1 Rh1 N3 60.15(17) . . ?
C1 Rh1 P1 95.95(17) . . ?
N1 Rh1 P1 90.53(13) . . ?
N3 Rh1 P1 88.73(12) . . ?
C1 Rh1 I2 84.96(17) . . ?
N1 Rh1 I2 167.25(13) . . ?
N3 Rh1 I2 107.57(13) . . ?
P1 Rh1 I2 92.67(4) . . ?
C1 Rh1 I1 84.18(17) . . ?
N1 Rh1 I1 86.69(13) . . ?
N3 Rh1 I1 90.51(12) . . ?
P1 Rh1 I1 177.13(4) . . ?
I2 Rh1 I1 90.20(2) . . ?
O1 C1 Rh1 176.7(5) . . ?
C37 P1 C31 107.2(3) . . ?
C37 P1 C25 105.0(3) . . ?
C31 P1 C25 103.6(3) . . ?
C37 P1 Rh1 110.97(18) . . ?
C31 P1 Rh1 112.35(19) . . ?
C25 P1 Rh1 116.97(19) . . ?
N2 N1 C11 119.0(5) . . ?
N2 N1 Rh1 99.6(3) . . ?
C11 N1 Rh1 140.8(4) . . ?
N1 N2 N3 103.7(4) . . ?
N2 N3 C18 116.6(5) . . ?
N2 N3 Rh1 96.4(3) . . ?
C18 N3 Rh1 146.8(4) . . ?
C16 C11 C12 118.9(6) . . ?
C16 C11 N1 119.0(5) . . ?
C12 C11 N1 122.0(5) . . ?
C13 C12 C11 119.9(6) . . ?
C12 C13 C14 122.5(6) . . ?
C15 C14 C13 116.5(6) . . ?
C15 C14 C17 121.5(6) . . ?
C13 C14 C17 122.0(6) . . ?
C14 C15 C16 122.6(6) . . ?
C11 C16 C15 119.6(6) . . ?
C23 C18 C19 120.2(6) . . ?
C23 C18 N3 118.5(6) . . ?
C19 C18 N3 121.3(6) . . ?
C20 C19 C18 119.0(6) . . ?
C21 C20 C19 121.8(7) . . ?
C20 C21 C22 118.2(6) . . ?
C20 C21 C24 121.3(7) . . ?
C22 C21 C24 120.5(8) . . ?
C21 C22 C23 121.2(7) . . ?
C18 C23 C22 119.6(6) . . ?
C26 C25 C30 119.3(5) . . ?
C26 C25 P1 121.3(4) . . ?
C30 C25 P1 119.3(5) . . ?
C27 C26 C25 120.5(6) . . ?
C28 C27 C26 119.9(6) . . ?
C29 C28 C27 120.3(6) . . ?
C28 C29 C30 120.5(6) . . ?
C29 C30 C25 119.5(6) . . ?
C36 C31 C32 118.0(5) . . ?
C36 C31 P1 123.7(4) . . ?
C32 C31 P1 118.2(4) . . ?
C33 C32 C31 121.2(5) . . ?
C34 C33 C32 120.0(6) . . ?
C35 C34 C33 119.2(6) . . ?
C34 C35 C36 121.2(6) . . ?
C31 C36 C35 120.4(6) . . ?
C42 C37 C38 118.3(5) . . ?
C42 C37 P1 121.4(4) . . ?
C38 C37 P1 120.2(4) . . ?
C39 C38 C37 120.2(5) . . ?
C38 C39 C40 121.2(6) . . ?
C39 C40 C41 119.2(6) . . ?
C42 C41 C40 120.0(6) . . ?
C41 C42 C37 121.1(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C1 1.879(6) . ?
Rh1 N1 2.050(5) . ?
Rh1 N3 2.097(5) . ?
Rh1 P1 2.3610(16) . ?
Rh1 I2 2.6778(7) . ?
Rh1 I1 2.7010(8) . ?
C1 O1 1.113(6) . ?
P1 C37 1.810(5) . ?
P1 C31 1.812(5) . ?
P1 C25 1.822(6) . ?
N1 N2 1.307(6) . ?
N1 C11 1.420(7) . ?
N2 N3 1.336(6) . ?
N3 C18 1.408(7) . ?
C11 C16 1.370(7) . ?
C11 C12 1.389(8) . ?
C12 C13 1.370(8) . ?
C13 C14 1.378(8) . ?
C14 C15 1.372(8) . ?
C14 C17 1.504(8) . ?
C15 C16 1.385(7) . ?
C18 C23 1.370(8) . ?
C18 C19 1.397(8) . ?
C19 C20 1.393(8) . ?
C20 C21 1.372(9) . ?
C21 C22 1.387(9) . ?
C21 C24 1.500(9) . ?
C22 C23 1.400(8) . ?
C25 C26 1.391(8) . ?
C25 C30 1.400(7) . ?
C26 C27 1.384(7) . ?
C27 C28 1.382(8) . ?
C28 C29 1.377(9) . ?
C29 C30 1.390(8) . ?
C31 C36 1.377(7) . ?
C31 C32 1.395(7) . ?
C32 C33 1.394(7) . ?
C33 C34 1.374(8) . ?
C34 C35 1.370(8) . ?
C35 C36 1.397(8) . ?
C37 C42 1.393(7) . ?
C37 C38 1.401(7) . ?
C38 C39 1.370(7) . ?
C39 C40 1.382(8) . ?
C40 C41 1.390(8) . ?
C41 C42 1.377(7) . ?
