#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:55:00 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180202 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/96/7109688.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_7109688
loop_
_publ_author_name
'Ming-Chuan Cheng'
'Chi-Lun Mai'
'Chen-Yu Yeh'
'Gene-Hsiang Lee'
'Shie-Ming Peng'
_publ_section_title
;
 Facile synthesis of heterotrimetallic metal-string complex
 [NiCoRh(dpa)4Cl2] through direct metal replacement
;
_journal_name_full               Chem.Commun.
_journal_page_first              7938
_journal_paper_doi               10.1039/c3cc43909g
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C42 H36 Cl5 Co F6 N12 Ni P Rh'
_chemical_formula_weight         1251.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 110.081(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7300(10)
_cell_length_b                   17.2013(8)
_cell_length_c                   15.5306(8)
_cell_measurement_reflns_used    17281
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.66
_cell_volume                     4699.5(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_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      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω 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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17281
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.176
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0754P)²+6.7405P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1533
_reflns_number_gt                3675
_reflns_number_total             5347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43909g.txt
_cod_data_source_block           ic15630
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7109688
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Rh Rh 0.0000 0.36574(3) 0.2500 0.02826(15) Uani 1 2 d S
Ni Ni 0.0000 0.09466(4) 0.2500 0.0273(2) Uani 1 2 d S
Co Co 0.0000 0.22988(4) 0.2500 0.0251(2) Uani 1 2 d S
Cl1 Cl 0.0000 0.51554(9) 0.2500 0.0391(4) Uani 1 2 d S
N1 N 0.1097(2) 0.3582(2) 0.2477(3) 0.0304(8) Uani 1 1 d .
N2 N 0.0853(2) 0.2280(2) 0.2088(3) 0.0369(9) Uani 1 1 d .
N3 N 0.0536(2) 0.0997(2) 0.1642(3) 0.0317(8) Uani 1 1 d .
N4 N 0.0437(2) 0.3574(2) 0.3943(2) 0.0304(8) Uani 1 1 d .
N5 N 0.0669(2) 0.2265(2) 0.3763(3) 0.0376(9) Uani 1 1 d .
N6 N 0.0958(2) 0.09921(19) 0.3481(3) 0.0318(8) Uani 1 1 d .
C1 C 0.1569(3) 0.4199(3) 0.2666(4) 0.0407(12) Uani 1 1 d .
H1 H 0.1375 0.4688 0.2765 0.049 Uiso 1 1 calc R
C2 C 0.2313(3) 0.4157(3) 0.2724(4) 0.0472(13) Uani 1 1 d .
H2 H 0.2617 0.4613 0.2821 0.057 Uiso 1 1 calc R
C3 C 0.2615(3) 0.3438(3) 0.2636(3) 0.0427(12) Uani 1 1 d .
H3 H 0.3136 0.3389 0.2701 0.051 Uiso 1 1 calc R
C4 C 0.2150(3) 0.2798(3) 0.2455(4) 0.0417(12) Uani 1 1 d .
H4 H 0.2353 0.2298 0.2418 0.050 Uiso 1 1 calc R
C5 C 0.1373(3) 0.2882(3) 0.2324(4) 0.0387(11) Uani 1 1 d .
C6 C 0.0919(3) 0.1658(3) 0.1561(3) 0.0380(11) Uani 1 1 d .
C7 C 0.1296(3) 0.1665(3) 0.0907(4) 0.0448(12) Uani 1 1 d .
H7 H 0.1540 0.2127 0.0820 0.054 Uiso 1 1 calc R
C8 C 0.1314(3) 0.1017(3) 0.0400(3) 0.0426(12) Uani 1 1 d .
H8 H 0.1549 0.1033 -0.0053 0.051 Uiso 1 1 calc R
C9 C 0.0981(3) 0.0341(3) 0.0563(3) 0.0420(12) Uani 1 1 d .
H9 H 0.1024 -0.0129 0.0265 0.050 Uiso 1 1 calc R
C10 C 0.0592(3) 0.0362(3) 0.1158(3) 0.0406(12) Uani 1 1 d .
H10 H 0.0343 -0.0100 0.1238 0.049 Uiso 1 1 calc R
C11 C 0.0499(3) 0.4194(3) 0.4493(3) 0.0374(11) Uani 1 1 d .
H11 H 0.0380 0.4691 0.4216 0.045 Uiso 1 1 calc R
C12 C 0.0726(3) 0.4148(3) 0.5441(3) 0.0424(12) Uani 1 1 d .
H12 H 0.0779 0.4607 0.5799 0.051 Uiso 1 1 calc R
C13 C 0.0876(3) 0.3427(3) 0.5860(3) 0.0422(12) Uani 1 1 d .
H13 H 0.0997 0.3376 0.6504 0.051 Uiso 1 1 calc R
C14 C 0.0846(3) 0.2790(3) 0.5319(3) 0.0429(12) Uani 1 1 d .
H14 H 0.0945 0.2289 0.5591 0.051 Uiso 1 1 calc R
C15 C 0.0667(3) 0.2868(3) 0.4350(3) 0.0376(11) Uani 1 1 d .
C16 C 0.1157(3) 0.1644(3) 0.4027(3) 0.0385(11) Uani 1 1 d .
C17 C 0.1881(3) 0.1664(3) 0.4746(4) 0.0433(12) Uani 1 1 d .
H17 H 0.2020 0.2094 0.5153 0.052 Uiso 1 1 calc R
C18 C 0.2373(3) 0.1052(3) 0.4839(3) 0.0428(12) Uani 1 1 d .
H18 H 0.2866 0.1076 0.5291 0.051 Uiso 1 1 calc R
C19 C 0.2163(3) 0.0408(3) 0.4290(4) 0.0431(12) Uani 1 1 d .
H19 H 0.2500 -0.0019 0.4363 0.052 Uiso 1 1 calc R
C20 C 0.1449(3) 0.0399(3) 0.3631(3) 0.0390(11) Uani 1 1 d .
H20 H 0.1297 -0.0052 0.3261 0.047 Uiso 1 1 calc R
P1 P 0.0000 -0.15711(10) 0.2500 0.0428(5) Uani 1 2 d S
F1 F 0.0000 -0.0630(2) 0.2500 0.0463(10) Uani 1 2 d S
F2 F 0.0000 -0.2503(2) 0.2500 0.0684(14) Uani 1 2 d S
F3 F -0.08521(18) -0.15596(17) 0.1792(2) 0.0627(9) Uani 1 1 d .
F4 F -0.0301(2) -0.15590(19) 0.3353(2) 0.0677(10) Uani 1 1 d .
C21 C 0.3950(3) 0.1582(3) 0.0907(4) 0.0538(14) Uani 1 1 d .
H21A H 0.4405 0.1296 0.1297 0.065 Uiso 1 1 calc R
H21B H 0.4085 0.2139 0.0916 0.065 Uiso 1 1 calc R
Cl2 Cl 0.32102(11) 0.14688(17) 0.13530(16) 0.1166(9) Uani 1 1 d .
Cl3 Cl 0.36736(9) 0.12254(8) -0.02340(10) 0.0590(4) Uani 1 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'
F F 0.0171 0.0103 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
_geom_angle_site_symmetry_3
N1 Rh N1 172.81(19) 2 .
N1 Rh N4 90.17(14) 2 .
N1 Rh N4 89.35(14) . .
N1 Rh N4 89.34(14) 2 2
N1 Rh N4 90.17(14) . 2
N4 Rh N4 172.22(19) . 2
N1 Rh Co 86.40(9) 2 .
N1 Rh Co 86.41(9) . .
N4 Rh Co 86.11(9) . .
N4 Rh Co 86.11(9) 2 .
N1 Rh Cl1 93.60(9) 2 .
N1 Rh Cl1 93.59(9) . .
N4 Rh Cl1 93.89(9) . .
N4 Rh Cl1 93.89(9) 2 .
Co Rh Cl1 180.0 . .
N6 Ni N6 175.3(2) 2 .
N6 Ni N3 88.85(16) 2 2
N6 Ni N3 90.94(16) . 2
N6 Ni N3 90.94(16) 2 .
N6 Ni N3 88.85(16) . .
N3 Ni N3 174.9(2) 2 .
N6 Ni Co 87.66(10) 2 .
N6 Ni Co 87.66(10) . .
N3 Ni Co 87.45(10) 2 .
N3 Ni Co 87.45(10) . .
N2 Co N2 178.0(2) 2 .
N2 Co N5 90.82(17) 2 2
N2 Co N5 89.12(17) . 2
N2 Co N5 89.12(17) 2 .
N2 Co N5 90.82(17) . .
N5 Co N5 176.5(2) 2 .
N2 Co Ni 89.01(11) 2 .
N2 Co Ni 89.01(11) . .
N5 Co Ni 88.25(11) 2 .
N5 Co Ni 88.26(11) . .
N2 Co Rh 90.99(11) 2 .
N2 Co Rh 90.99(11) . .
N5 Co Rh 91.75(11) 2 .
N5 Co Rh 91.74(11) . .
Ni Co Rh 180.0 . .
C1 N1 C5 118.3(4) . .
C1 N1 Rh 121.8(3) . .
C5 N1 Rh 119.8(3) . .
C6 N2 C5 122.6(4) . .
C6 N2 Co 117.8(3) . .
C5 N2 Co 119.5(3) . .
C10 N3 C6 118.4(4) . .
C10 N3 Ni 120.6(3) . .
C6 N3 Ni 120.9(3) . .
C11 N4 C15 117.7(4) . .
C11 N4 Rh 122.6(3) . .
C15 N4 Rh 119.8(3) . .
C16 N5 C15 122.6(4) . .
C16 N5 Co 117.4(3) . .
C15 N5 Co 120.0(3) . .
C20 N6 C16 119.2(4) . .
C20 N6 Ni 120.5(3) . .
C16 N6 Ni 120.3(3) . .
N1 C1 C2 123.4(5) . .
C1 C2 C3 118.8(4) . .
C4 C3 C2 119.0(5) . .
C3 C4 C5 120.0(5) . .
N1 C5 N2 115.6(4) . .
N1 C5 C4 120.0(4) . .
N2 C5 C4 124.2(4) . .
N3 C6 N2 115.6(4) . .
N3 C6 C7 118.4(4) . .
N2 C6 C7 125.8(4) . .
C8 C7 C6 121.3(5) . .
C7 C8 C9 118.5(5) . .
C10 C9 C8 118.9(4) . .
N3 C10 C9 124.2(4) . .
N4 C11 C12 123.9(4) . .
C13 C12 C11 119.2(4) . .
C14 C13 C12 118.0(5) . .
C13 C14 C15 121.0(5) . .
N4 C15 N5 115.7(4) . .
N4 C15 C14 119.4(4) . .
N5 C15 C14 124.8(4) . .
N5 C16 N6 115.9(4) . .
N5 C16 C17 124.8(4) . .
N6 C16 C17 118.9(4) . .
C18 C17 C16 119.1(5) . .
C19 C18 C17 121.0(5) . .
C18 C19 C20 118.0(4) . .
N6 C20 C19 123.7(4) . .
F3 P1 F3 178.6(2) 2 .
F3 P1 F2 90.71(12) 2 .
F3 P1 F2 90.71(12) . .
F3 P1 F4 89.04(19) 2 .
F3 P1 F4 90.94(19) . .
F2 P1 F4 90.74(13) . .
F3 P1 F4 90.94(19) 2 2
F3 P1 F4 89.04(19) . 2
F2 P1 F4 90.74(13) . 2
F4 P1 F4 178.5(3) . 2
F3 P1 F1 89.29(12) 2 .
F3 P1 F1 89.29(12) . .
F2 P1 F1 180.0 . .
F4 P1 F1 89.26(13) . .
F4 P1 F1 89.26(13) 2 .
Cl2 C21 Cl3 110.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh N1 2.072(4) 2
Rh N1 2.072(4) .
Rh N4 2.110(4) .
Rh N4 2.110(4) 2
Rh Co 2.3371(8) .
Rh Cl1 2.5767(16) .
Ni N6 1.916(4) 2
Ni N6 1.916(4) .
Ni N3 1.925(4) 2
Ni N3 1.925(4) .
Ni Co 2.3259(10) .
Co N2 1.914(4) 2
Co N2 1.914(4) .
Co N5 1.932(4) 2
Co N5 1.932(4) .
N1 C1 1.347(6) .
N1 C5 1.364(6) .
N2 C6 1.378(6) .
N2 C5 1.383(6) .
N3 C10 1.350(6) .
N3 C6 1.374(6) .
N4 C11 1.346(5) .
N4 C15 1.369(6) .
N5 C16 1.374(6) .
N5 C15 1.382(6) .
N6 C20 1.339(5) .
N6 C16 1.377(6) .
C1 C2 1.367(7) .
C2 C3 1.386(7) .
C3 C4 1.372(7) .
C4 C5 1.405(6) .
C6 C7 1.423(7) .
C7 C8 1.371(7) .
C8 C9 1.383(7) .
C9 C10 1.360(7) .
C11 C12 1.387(7) .
C12 C13 1.384(7) .
C13 C14 1.371(7) .
C14 C15 1.431(7) .
C16 C17 1.431(7) .
C17 C18 1.372(7) .
C18 C19 1.370(7) .
C19 C20 1.377(6) .
P1 F3 1.597(3) 2
P1 F3 1.597(3) .
P1 F2 1.602(5) .
P1 F4 1.609(3) .
P1 F4 1.609(3) 2
P1 F1 1.619(4) .
C21 Cl2 1.760(6) .
C21 Cl3 1.776(6) .
