#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:20:33 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178646 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/57/4075789.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_4075789
loop_
_publ_author_name
'Lee, Chrong-Ching'
'Lin, Ying-Chih'
'Liu, Yi-Hung'
'Wang, Yu'
_publ_section_title
;
 Rhodium-Catalyzed Dimerization of Terminal Alkynes Assisted by MeI
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              136
_journal_paper_doi               10.1021/om049604s
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C49 H40 Cl4 I N2 O3 P2 Rh'
_chemical_formula_weight         1138.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                77.06(2)
_cell_angle_beta                 71.678(13)
_cell_angle_gamma                66.884(15)
_cell_formula_units_Z            2
_cell_length_a                   12.915(2)
_cell_length_b                   13.210(3)
_cell_length_c                   15.975(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      11.87
_cell_measurement_theta_min      7.8
_cell_volume                     2363.7(8)
_computing_cell_refinement       'Nonius EXPRESS'
_computing_data_collection       'Nonius EXPRESS'
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       'θ/2θ 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8309
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        <4
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  0.7785
_exptl_absorpt_correction_T_min  0.6829
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0000(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.943
_refine_ls_goodness_of_fit_obs   1.007
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         8309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.943
_refine_ls_restrained_S_obs      1.007
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_obs          0.0454
_refine_ls_shift/esd_max         -2.313
_refine_ls_shift/esd_mean        0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1475
_refine_ls_wR_factor_obs         0.1301
_reflns_number_observed          5793
_reflns_number_total             8309
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om049604ssi20040603_063631.cif
_cod_data_source_block           ic6186
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2363.9(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075789
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
Rh Rh 0.24328(3) 0.19492(3) 0.22492(3) 0.03252(14) Uani 1 d
I I 0.35165(3) 0.21445(4) 0.04387(2) 0.0504(2) Uani 1 d
P1 P 0.10066(11) 0.15295(11) 0.18727(9) 0.0340(3) Uani 1 d
P2 P 0.40819(13) 0.20459(13) 0.25709(9) 0.0397(3) Uani 1 d
O1 O 0.1372(5) 0.4461(4) 0.1826(4) 0.0714(14) Uani 1 d
O2 O 0.6677(6) -0.5715(5) 0.2690(5) 0.117(3) Uani 1 d
O3 O 0.5627(6) -0.5784(4) 0.4003(4) 0.093(2) Uani 1 d
N1 N 0.1196(6) 0.3829(6) 0.4166(4) 0.080(2) Uani 1 d
N2 N 0.5924(6) -0.5270(5) 0.3297(5) 0.072(2) Uani 1 d
C1 C 0.1411(5) 0.2067(5) 0.3594(3) 0.0415(13) Uani 1 d
C2 C 0.1295(5) 0.3033(6) 0.3924(4) 0.052(2) Uani 1 d
C3 C 0.1754(5) 0.3533(5) 0.1975(4) 0.0451(13) Uani 1 d
C4 C 0.3117(4) 0.0313(5) 0.2591(3) 0.0388(12) Uani 1 d
C5 C 0.3526(5) -0.0661(5) 0.2804(4) 0.0405(12) Uani 1 d
C6 C 0.4117(5) -0.1830(5) 0.2946(4) 0.0449(13) Uani 1 d
C7 C 0.5025(6) -0.2368(5) 0.2277(5) 0.065(2) Uani 1 d
C8 C 0.5618(6) -0.3486(6) 0.2382(5) 0.067(2) Uani 1 d
C9 C 0.5302(5) -0.4079(5) 0.3177(5) 0.054(2) Uani 1 d
C10 C 0.4379(7) -0.3580(5) 0.3845(4) 0.066(2) Uani 1 d
C11 C 0.3798(6) -0.2464(5) 0.3736(4) 0.061(2) Uani 1 d
C12 C 0.0164(5) 0.2677(5) 0.1201(4) 0.0410(13) Uani 1 d
C13 C -0.0515(5) 0.3660(5) 0.1565(4) 0.0485(14) Uani 1 d
C14 C -0.1161(6) 0.4561(6) 0.1069(5) 0.067(2) Uani 1 d
C15 C -0.1135(7) 0.4462(7) 0.0227(6) 0.076(2) Uani 1 d
C16 C -0.0440(8) 0.3490(8) -0.0149(5) 0.076(2) Uani 1 d
C17 C 0.0216(6) 0.2599(6) 0.0338(4) 0.055(2) Uani 1 d
C18 C -0.0072(5) 0.1176(4) 0.2838(3) 0.0360(12) Uani 1 d
C19 C -0.1233(5) 0.1847(5) 0.3074(4) 0.0458(14) Uani 1 d
C20 C -0.1979(5) 0.1548(6) 0.3839(4) 0.056(2) Uani 1 d
C21 C -0.1582(6) 0.0561(6) 0.4361(4) 0.058(2) Uani 1 d
C22 C -0.0447(6) -0.0116(6) 0.4121(4) 0.058(2) Uani 1 d
C23 C 0.0312(5) 0.0191(5) 0.3362(4) 0.0515(15) Uani 1 d
C24 C 0.1489(5) 0.0322(5) 0.1278(4) 0.0407(12) Uani 1 d
C25 C 0.0636(5) 0.0017(6) 0.1168(5) 0.056(2) Uani 1 d
C26 C 0.0907(6) -0.0901(7) 0.0760(5) 0.070(2) Uani 1 d
C27 C 0.2071(7) -0.1546(6) 0.0460(5) 0.066(2) Uani 1 d
C28 C 0.2942(6) -0.1252(5) 0.0570(4) 0.055(2) Uani 1 d
C29 C 0.2648(5) -0.0317(5) 0.0969(4) 0.0422(13) Uani 1 d
C30 C 0.4369(6) 0.3318(6) 0.2069(4) 0.054(2) Uani 1 d
C31 C 0.5355(7) 0.3306(6) 0.1375(5) 0.066(2) Uani 1 d
C32 C 0.5546(9) 0.4268(8) 0.0957(6) 0.089(3) Uani 1 d
C33 C 0.4766(12) 0.5258(9) 0.1219(7) 0.102(3) Uani 1 d
C34 C 0.3763(10) 0.5314(7) 0.1895(7) 0.092(3) Uani 1 d
C35 C 0.3583(8) 0.4321(6) 0.2336(5) 0.073(2) Uani 1 d
C36 C 0.3971(5) 0.1960(5) 0.3756(4) 0.0436(13) Uani 1 d
C37 C 0.3769(6) 0.1035(6) 0.4301(4) 0.056(2) Uani 1 d
C38 C 0.3697(7) 0.0920(7) 0.5202(4) 0.072(2) Uani 1 d
C39 C 0.3831(8) 0.1706(8) 0.5546(5) 0.080(2) Uani 1 d
C40 C 0.4070(8) 0.2571(8) 0.5017(6) 0.082(2) Uani 1 d
C41 C 0.4143(7) 0.2712(7) 0.4119(5) 0.068(2) Uani 1 d
C42 C 0.5498(5) 0.0946(5) 0.2233(4) 0.0416(13) Uani 1 d
C43 C 0.5724(5) 0.0219(5) 0.1642(4) 0.0484(14) Uani 1 d
C44 C 0.6822(6) -0.0582(6) 0.1423(5) 0.060(2) Uani 1 d
C45 C 0.7674(5) -0.0666(7) 0.1803(5) 0.066(2) Uani 1 d
C46 C 0.7468(6) 0.0063(7) 0.2368(5) 0.066(2) Uani 1 d
C47 C 0.6378(5) 0.0878(6) 0.2591(4) 0.059(2) Uani 1 d
Cl1 Cl -0.1480 0.6219 0.2933 0.254 Uani 1 d
Cl3 Cl -0.1866 0.4353 0.4198 0.354 Uani 1 d
Cl2 Cl 0.0181 0.7238 0.2850 0.453 Uani 1 d
Cl4 Cl 0.1316 0.6685 0.3944 0.549 Uani 1 d
C48 C -0.0861 0.6080 0.3791 0.410 Uani 1 d
C49 C 0.1512 0.6679 0.5150 0.172 Uani 1 d
H1A H 0.1837 0.1477 0.3955 0.054 Uiso 1 d
H1B H 0.0681 0.2023 0.3585 0.054 Uiso 1 d
H7 H 0.5247 -0.1945 0.1715 0.066 Uiso 1 d
H8 H 0.6245 -0.3849 0.1907 0.070 Uiso 1 d
H10 H 0.4146 -0.4029 0.4390 0.071 Uiso 1 d
H11 H 0.3157 -0.2114 0.4207 0.067 Uiso 1 d
H13 H -0.0529 0.3734 0.2158 0.056 Uiso 1 d
H14 H -0.1639 0.5257 0.1329 0.071 Uiso 1 d
H15 H -0.1606 0.5070 -0.0107 0.083 Uiso 1 d
H16 H -0.0425 0.3436 -0.0743 0.081 Uiso 1 d
H17 H 0.0714 0.1909 0.0073 0.071 Uiso 1 d
H19 H -0.1517 0.2536 0.2704 0.055 Uiso 1 d
H20 H -0.2785 0.2025 0.4019 0.065 Uiso 1 d
H21 H -0.2113 0.0346 0.4877 0.068 Uiso 1 d
H22 H -0.0169 -0.0810 0.4485 0.069 Uiso 1 d
H23 H 0.1119 -0.0287 0.3197 0.059 Uiso 1 d
H25 H -0.0178 0.0479 0.1373 0.069 Uiso 1 d
H26 H 0.0297 -0.1103 0.0678 0.082 Uiso 1 d
H27 H 0.2283 -0.2190 0.0178 0.080 Uiso 1 d
H28 H 0.3740 -0.1705 0.0366 0.065 Uiso 1 d
H29 H 0.3256 -0.0109 0.1032 0.055 Uiso 1 d
H31 H 0.5926 0.2587 0.1202 0.082 Uiso 1 d
H32 H 0.6251 0.4260 0.0489 0.108 Uiso 1 d
H33 H 0.4869 0.5947 0.0953 0.122 Uiso 1 d
H34 H 0.3170 0.6027 0.2093 0.110 Uiso 1 d
H35 H 0.2872 0.4347 0.2820 0.090 Uiso 1 d
H37 H 0.3669 0.0485 0.4051 0.065 Uiso 1 d
H38 H 0.3538 0.0288 0.5589 0.083 Uiso 1 d
H39 H 0.3748 0.1640 0.6183 0.092 Uiso 1 d
H40 H 0.4211 0.3093 0.5279 0.099 Uiso 1 d
H41 H 0.4310 0.3365 0.3739 0.084 Uiso 1 d
H43 H 0.5118 0.0277 0.1383 0.061 Uiso 1 d
H44 H 0.6975 -0.1092 0.1012 0.069 Uiso 1 d
H45 H 0.8424 -0.1251 0.1667 0.073 Uiso 1 d
H46 H 0.8075 0.0019 0.2629 0.076 Uiso 1 d
H47 H 0.6244 0.1404 0.2978 0.070 Uiso 1 d
H49A H -0.0464(186) 0.7202(177) 0.4414(136) 0.364(117) Uiso 1 d
H49B H 0.2882(153) 0.8931(140) 0.1963(112) 0.288(82) Uiso 1 d
H48A H -0.5885(129) 0.8442(122) 0.6261(97) 0.241(65) Uiso 1 d
H48B H -0.1353(45) 0.5500(42) 0.4104(34) 0.040(15) Uiso 1 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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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'
Rh Rh -1.1178 0.9187 '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
C3 Rh C4 177.5(2) .
C3 Rh C1 90.2(2) .
C4 Rh C1 87.4(2) .
C3 Rh P1 95.1(2) .
C4 Rh P1 85.8(2) .
C1 Rh P1 90.6(2) .
C3 Rh P2 94.0(2) .
C4 Rh P2 85.3(2) .
C1 Rh P2 93.5(2) .
P1 Rh P2 169.92(5) .
C3 Rh I 80.8(2) .
C4 Rh I 101.63(15) .
C1 Rh I 170.6(2) .
P1 Rh I 87.75(4) .
P2 Rh I 89.57(4) .
C12 P1 C24 104.7(3) .
C12 P1 C18 105.5(2) .
C24 P1 C18 99.6(2) .
C12 P1 Rh 113.0(2) .
C24 P1 Rh 118.5(2) .
C18 P1 Rh 113.9(2) .
C30 P2 C36 105.4(3) .
C30 P2 C42 103.9(3) .
C36 P2 C42 100.4(3) .
C30 P2 Rh 113.1(2) .
C36 P2 Rh 114.7(2) .
C42 P2 Rh 117.8(2) .
O2 N2 O3 122.2(7) .
O2 N2 C9 119.6(7) .
O3 N2 C9 118.2(7) .
C2 C1 Rh 112.6(4) .
N1 C2 C1 177.9(7) .
O1 C3 Rh 178.4(5) .
C5 C4 Rh 179.2(5) .
C4 C5 C6 172.4(6) .
C7 C6 C11 118.0(6) .
C7 C6 C5 119.9(5) .
C11 C6 C5 122.1(5) .
C8 C7 C6 122.0(6) .
C9 C8 C7 118.5(6) .
C8 C9 C10 121.1(6) .
C8 C9 N2 119.1(6) .
C10 C9 N2 119.8(6) .
C11 C10 C9 119.9(6) .
C10 C11 C6 120.4(6) .
C17 C12 C13 119.6(6) .
C17 C12 P1 122.0(5) .
C13 C12 P1 118.4(4) .
C12 C13 C14 120.2(6) .
C15 C14 C13 119.7(7) .
C14 C15 C16 120.5(6) .
C15 C16 C17 119.8(7) .
C12 C17 C16 120.1(7) .
C23 C18 C19 118.8(5) .
C23 C18 P1 117.4(4) .
C19 C18 P1 123.9(4) .
C20 C19 C18 120.3(5) .
C21 C20 C19 120.3(6) .
C22 C21 C20 119.6(6) .
C21 C22 C23 120.3(6) .
C18 C23 C22 120.6(6) .
C25 C24 C29 118.9(5) .
C25 C24 P1 117.2(4) .
C29 C24 P1 123.8(4) .
C26 C25 C24 121.7(6) .
C25 C26 C27 119.1(6) .
C26 C27 C28 119.8(6) .
C29 C28 C27 120.0(6) .
C28 C29 C24 120.4(5) .
C35 C30 C31 118.7(6) .
C35 C30 P2 120.3(5) .
C31 C30 P2 121.0(5) .
C32 C31 C30 121.4(8) .
C33 C32 C31 119.8(8) .
C32 C33 C34 120.9(8) .
C33 C34 C35 119.0(9) .
C30 C35 C34 120.0(8) .
C41 C36 C37 118.9(6) .
C41 C36 P2 123.8(5) .
C37 C36 P2 117.2(5) .
C38 C37 C36 119.5(7) .
C39 C38 C37 119.9(7) .
C40 C39 C38 120.6(7) .
C39 C40 C41 120.9(8) .
C36 C41 C40 120.1(7) .
C43 C42 C47 119.6(6) .
C43 C42 P2 123.7(4) .
C47 C42 P2 116.7(5) .
C42 C43 C44 119.6(6) .
C45 C44 C43 120.3(6) .
C46 C45 C44 120.4(6) .
C45 C46 C47 120.2(6) .
C42 C47 C46 119.7(6) .
C49 Cl4 Cl2 152.855(8) .
Cl3 C49 Cl4 125.002(14) 2_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh C3 1.931(6) .
Rh C4 2.007(6) .
Rh C1 2.142(5) .
Rh P1 2.3896(14) .
Rh P2 2.3976(15) .
Rh I 2.7920(8) .
P1 C12 1.829(6) .
P1 C24 1.834(6) .
P1 C18 1.837(5) .
P2 C30 1.817(6) .
P2 C36 1.833(6) .
P2 C42 1.841(6) .
O1 C3 1.128(7) .
O2 N2 1.202(9) .
O3 N2 1.213(8) .
N1 C2 1.147(8) .
N2 C9 1.457(8) .
C1 C2 1.425(9) .
C4 C5 1.197(8) .
C5 C6 1.431(8) .
C6 C7 1.385(9) .
C6 C11 1.391(8) .
C7 C8 1.370(9) .
C8 C9 1.369(9) .
C9 C10 1.376(10) .
C10 C11 1.366(9) .
C12 C17 1.384(8) .
C12 C13 1.385(8) .
C13 C14 1.397(9) .
C14 C15 1.369(12) .
C15 C16 1.384(12) .
C16 C17 1.389(10) .
C18 C23 1.381(8) .
C18 C19 1.388(8) .
C19 C20 1.386(8) .
C20 C21 1.385(9) .
C21 C22 1.366(9) .
C22 C23 1.393(9) .
C24 C25 1.381(8) .
C24 C29 1.388(8) .
C25 C26 1.377(9) .
C26 C27 1.393(10) .
C27 C28 1.394(10) .
C28 C29 1.381(8) .
C30 C35 1.376(10) .
C30 C31 1.398(10) .
C31 C32 1.372(11) .
C32 C33 1.358(14) .
C33 C34 1.390(14) .
C34 C35 1.413(11) .
C36 C41 1.374(9) .
C36 C37 1.396(9) .
C37 C38 1.391(9) .
C38 C39 1.366(11) .
C39 C40 1.340(12) .
C40 C41 1.382(10) .
C42 C43 1.383(8) .
C42 C47 1.390(8) .
C43 C44 1.389(9) .
C44 C45 1.371(10) .
C45 C46 1.362(10) .
C46 C47 1.390(9) .
Cl1 C48 1.7358(3) .
Cl3 C49 1.5255(4) 2_566
Cl2 Cl4 2.4355(4) .
Cl4 C49 2.0190(4) .
C49 Cl3 1.5255(4) 2_566
