#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/57/4075768.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_4075768
loop_
_publ_author_name
'Tanaka, Shukichi'
'Dubs, Christian'
'Inagaki, Akiko'
'Akita, Munetaka'
_publ_section_title
;
 Polynuclear Rhodium Complexes with Dinucleating PNNP Ligand: 
 Dynamic and Diverse M···M Interactions in
 [(μ-X)Rh2(PNNP)(CO)2]n+and [(μ4-X)Rh4(PNNP)2(CO)4]n+[X = H, O,
 C⋮C−R, R−C⋮C−R, C⋮C, CHCH2,
 SMe2;n= 0, 1:  PNNP = 3,5-bis(diphenylphosphinomethyl)pyrazolato]
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              163
_journal_paper_doi               10.1021/om049427v
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C33 H26 N2 O2 P2 Rh2 '
_chemical_formula_sum            'C33 H26 N2 O2 P2 Rh2'
_chemical_formula_weight         750.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 91.523(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9921(4)
_cell_length_b                   14.4141(8)
_cell_length_c                   17.4658(9)
_cell_measurement_reflns_used    21254
_cell_measurement_temperature    213.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     3018.0(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS86
_diffrn_detector_area_resol_mean 10.00
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23371
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.41
_refine_diff_density_min         -1.49
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.791
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5768
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          -0.0020
_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_ref         0.0960
_reflns_number_gt                5768
_reflns_number_total             6234
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            om049427vsi20040726_024341.cif
_cod_data_source_block           compound_2a
_cod_original_formula_sum        'C33 H26 N2 O2 P2 Rh2 '
_cod_database_code               4075768
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
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_calc_flag
Rh(1) Rh 0.26721(1) 0.63964(1) 0.19880(1) 0.02444(8) Uani 1.00 d
Rh(2) Rh 0.48698(1) 0.66497(1) 0.35593(1) 0.02460(8) Uani 1.00 d
P(1) P 0.22200(5) 0.71748(4) 0.08848(3) 0.0269(1) Uani 1.00 d
P(2) P 0.62217(5) 0.76733(4) 0.37901(3) 0.0303(1) Uani 1.00 d
O(01) O 0.0809(2) 0.5044(2) 0.1927(1) 0.0547(6) Uani 1.00 d
O(02) O 0.5993(2) 0.5529(2) 0.4776(1) 0.0661(7) Uani 1.00 d
N(1) N 0.3849(2) 0.7406(1) 0.2048(1) 0.0258(4) Uani 1.00 d
N(2) N 0.4551(2) 0.7546(1) 0.2661(1) 0.0271(4) Uani 1.00 d
C(1) C 0.3227(2) 0.5923(2) 0.3025(1) 0.0275(4) Uani 1.00 d
C(01) C 0.1539(2) 0.5558(2) 0.1943(1) 0.0345(5) Uani 1.00 d
C(2) C 0.3416(2) 0.5627(2) 0.3666(2) 0.0326(5) Uani 1.00 d
C(02) C 0.5495(2) 0.5946(2) 0.4322(2) 0.0387(6) Uani 1.00 d
C(11) C 0.3990(2) 0.8093(2) 0.1540(1) 0.0299(5) Uani 1.00 d
C(12) C 0.4786(2) 0.8708(2) 0.1829(2) 0.0353(5) Uani 1.00 d
C(13) C 0.5121(2) 0.8334(2) 0.2532(2) 0.0319(5) Uani 1.00 d
C(14) C 0.3354(2) 0.8041(2) 0.0789(1) 0.0336(5) Uani 1.00 d
C(15) C 0.5942(3) 0.8656(2) 0.3135(2) 0.0460(7) Uani 1.00 d
C(21) C 0.0961(2) 0.7880(2) 0.0914(1) 0.0327(5) Uani 1.00 d
C(22) C 0.0399(3) 0.7946(3) 0.1597(2) 0.0518(8) Uani 1.00 d
C(23) C -0.0543(3) 0.8491(3) 0.1652(2) 0.069(1) Uani 1.00 d
C(24) C -0.0946(3) 0.8967(3) 0.1024(2) 0.0613(9) Uani 1.00 d
C(25) C -0.0397(3) 0.8907(3) 0.0342(2) 0.0594(9) Uani 1.00 d
C(26) C 0.0555(3) 0.8373(2) 0.0287(2) 0.0467(7) Uani 1.00 d
C(31) C 0.2116(2) 0.6567(2) -0.0032(1) 0.0302(5) Uani 1.00 d
C(32) C 0.1616(3) 0.5694(2) -0.0048(2) 0.0474(7) Uani 1.00 d
C(33) C 0.1515(3) 0.5192(2) -0.0724(2) 0.0588(9) Uani 1.00 d
C(34) C 0.1936(3) 0.5551(3) -0.1387(2) 0.0520(8) Uani 1.00 d
C(35) C 0.2424(2) 0.6409(3) -0.1384(2) 0.0494(8) Uani 1.00 d
C(36) C 0.2520(2) 0.6926(2) -0.0710(2) 0.0389(6) Uani 1.00 d
C(41) C 0.6241(2) 0.8135(2) 0.4761(2) 0.0352(5) Uani 1.00 d
C(42) C 0.5354(3) 0.8694(2) 0.4987(2) 0.0466(7) Uani 1.00 d
C(43) C 0.5264(3) 0.8950(2) 0.5743(2) 0.0586(9) Uani 1.00 d
C(44) C 0.6024(4) 0.8657(3) 0.6282(2) 0.0613(9) Uani 1.00 d
C(45) C 0.6899(3) 0.8107(3) 0.6075(2) 0.0584(8) Uani 1.00 d
C(46) C 0.7009(3) 0.7835(2) 0.5314(2) 0.0446(6) Uani 1.00 d
C(51) C 0.7639(2) 0.7323(2) 0.3620(1) 0.0373(6) Uani 1.00 d
C(52) C 0.8515(2) 0.7948(3) 0.3752(2) 0.0476(7) Uani 1.00 d
C(53) C 0.9607(3) 0.7677(3) 0.3618(2) 0.062(1) Uani 1.00 d
C(54) C 0.9826(3) 0.6810(4) 0.3352(2) 0.065(1) Uani 1.00 d
C(55) C 0.8971(3) 0.6183(3) 0.3210(2) 0.0593(9) Uani 1.00 d
C(56) C 0.7873(2) 0.6440(3) 0.3345(2) 0.0473(7) Uani 1.00 d
H(1) H 0.339(2) 0.528(2) 0.408(1) 0.02307(8) Uiso 1.00 calc
H(2) H 0.5033 0.9271 0.1593 0.0420 Uiso 1.00 calc
H(3) H 0.3849 0.7848 0.0395 0.0411 Uiso 1.00 calc
H(4) H 0.3054 0.8629 0.0655 0.0411 Uiso 1.00 calc
H(5) H 0.5660 0.9169 0.3408 0.0548 Uiso 1.00 calc
H(6) H 0.6625 0.8840 0.2900 0.0548 Uiso 1.00 calc
H(7) H 0.0684 0.7599 0.2034 0.0626 Uiso 1.00 calc
H(8) H -0.0915 0.8528 0.2142 0.0883 Uiso 1.00 calc
H(9) H -0.1619 0.9334 0.1038 0.0729 Uiso 1.00 calc
H(10) H -0.0682 0.9225 -0.0101 0.0719 Uiso 1.00 calc
H(11) H 0.0952 0.8362 -0.0184 0.0560 Uiso 1.00 calc
H(12) H 0.1345 0.5434 0.0419 0.0594 Uiso 1.00 calc
H(13) H 0.1139 0.4601 -0.0733 0.0684 Uiso 1.00 calc
H(14) H 0.1892 0.5199 -0.1857 0.0623 Uiso 1.00 calc
H(15) H 0.2708 0.6664 -0.1849 0.0584 Uiso 1.00 calc
H(16) H 0.2859 0.7535 -0.0710 0.0462 Uiso 1.00 calc
H(17) H 0.4819 0.8894 0.4604 0.0590 Uiso 1.00 calc
H(18) H 0.4653 0.9355 0.5877 0.0682 Uiso 1.00 calc
H(19) H 0.5952 0.8831 0.6817 0.0758 Uiso 1.00 calc
H(20) H 0.7455 0.7897 0.6450 0.0720 Uiso 1.00 calc
H(21) H 0.7615 0.7438 0.5170 0.0548 Uiso 1.00 calc
H(22) H 0.8360 0.8570 0.3932 0.0597 Uiso 1.00 calc
H(23) H 1.0207 0.8110 0.3715 0.0777 Uiso 1.00 calc
H(24) H 1.0581 0.6629 0.3250 0.0744 Uiso 1.00 calc
H(25) H 0.9132 0.5559 0.3027 0.0734 Uiso 1.00 calc
H(26) H 0.7280 0.6007 0.3243 0.0558 Uiso 1.00 calc
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)
;
O O 0.011 0.006
;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)
;
Rh Rh -1.118 0.919
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.102 0.094
;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
P(1) Rh(1) N(1) 80.80(5) yes
P(1) Rh(1) C(1) 169.37(7) yes
P(1) Rh(1) C(01) 97.46(8) yes
N(1) Rh(1) C(1) 89.10(8) yes
N(1) Rh(1) C(01) 175.77(10) yes
C(1) Rh(1) C(01) 92.4(1) yes
P(2) Rh(2) N(2) 80.88(5) yes
P(2) Rh(2) C(1) 161.59(6) yes
P(2) Rh(2) C(2) 164.70(7) yes
P(2) Rh(2) C(02) 87.31(9) yes
N(2) Rh(2) C(1) 80.99(8) yes
N(2) Rh(2) C(2) 109.79(8) yes
N(2) Rh(2) C(02) 166.24(10) yes
C(1) Rh(2) C(2) 29.89(8) yes
C(1) Rh(2) C(02) 111.1(1) yes
C(2) Rh(2) C(02) 83.2(1) yes
Rh(1) P(1) C(14) 104.40(8) yes
Rh(1) P(1) C(21) 115.42(8) yes
Rh(1) P(1) C(31) 120.88(8) yes
C(14) P(1) C(21) 103.7(1) yes
C(14) P(1) C(31) 106.0(1) yes
C(21) P(1) C(31) 104.8(1) yes
Rh(2) P(2) C(15) 106.11(10) yes
Rh(2) P(2) C(41) 113.77(9) yes
Rh(2) P(2) C(51) 118.03(10) yes
C(15) P(2) C(41) 107.1(1) yes
C(15) P(2) C(51) 105.6(1) yes
C(41) P(2) C(51) 105.5(1) yes
Rh(1) N(1) N(2) 124.3(1) yes
Rh(1) N(1) C(11) 126.5(1) yes
N(2) N(1) C(11) 108.9(2) yes
Rh(2) N(2) N(1) 127.2(1) yes
Rh(2) N(2) C(13) 124.8(2) yes
N(1) N(2) C(13) 107.5(2) yes
Rh(1) C(1) Rh(2) 116.5(1) yes
Rh(1) C(1) C(2) 171.7(2) yes
Rh(2) C(1) C(2) 70.3(1) yes
Rh(1) C(01) O(01) 178.1(2) yes
Rh(2) C(2) C(1) 79.8(2) yes
Rh(2) C(02) O(02) 173.1(3) yes
N(1) C(11) C(12) 109.2(2) yes
N(1) C(11) C(14) 118.0(2) yes
C(12) C(11) C(14) 132.7(2) yes
C(11) C(12) C(13) 104.7(2) yes
N(2) C(13) C(12) 109.8(2) yes
N(2) C(13) C(15) 118.1(2) yes
C(12) C(13) C(15) 132.1(2) yes
P(1) C(14) C(11) 108.1(2) yes
P(2) C(15) C(13) 107.6(2) yes
P(1) C(21) C(22) 118.9(2) yes
P(1) C(21) C(26) 122.6(2) yes
C(22) C(21) C(26) 118.5(3) yes
C(21) C(22) C(23) 120.9(3) yes
C(22) C(23) C(24) 120.1(3) yes
C(23) C(24) C(25) 119.6(3) yes
C(24) C(25) C(26) 120.6(3) yes
C(21) C(26) C(25) 120.3(3) yes
P(1) C(31) C(32) 118.1(2) yes
P(1) C(31) C(36) 123.4(2) yes
C(32) C(31) C(36) 118.5(2) yes
C(31) C(32) C(33) 121.0(3) yes
C(32) C(33) C(34) 119.7(3) yes
C(33) C(34) C(35) 120.2(3) yes
C(34) C(35) C(36) 120.7(3) yes
C(31) C(36) C(35) 119.8(3) yes
P(2) C(41) C(42) 118.8(2) yes
P(2) C(41) C(46) 121.8(2) yes
C(42) C(41) C(46) 118.6(3) yes
C(41) C(42) C(43) 120.2(3) yes
C(42) C(43) C(44) 120.9(3) yes
C(43) C(44) C(45) 119.9(3) yes
C(44) C(45) C(46) 120.5(3) yes
C(41) C(46) C(45) 119.8(3) yes
P(2) C(51) C(52) 119.9(2) yes
P(2) C(51) C(56) 120.8(2) yes
C(52) C(51) C(56) 119.3(2) yes
C(51) C(52) C(53) 119.8(3) yes
C(52) C(53) C(54) 120.4(3) yes
C(53) C(54) C(55) 120.8(3) yes
C(54) C(55) C(56) 119.6(4) yes
C(51) C(56) C(55) 120.1(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Rh(1) P(1) 2.2825(6) yes
Rh(1) N(1) 2.028(2) yes
Rh(1) C(1) 2.030(2) yes
Rh(1) C(01) 1.819(3) yes
Rh(2) P(2) 2.2210(6) yes
Rh(2) N(2) 2.061(2) yes
Rh(2) C(1) 2.399(2) yes
Rh(2) C(2) 2.294(2) yes
Rh(2) C(02) 1.820(3) yes
P(1) C(14) 1.857(3) yes
P(1) C(21) 1.822(3) yes
P(1) C(31) 1.826(3) yes
P(2) C(15) 1.846(3) yes
P(2) C(41) 1.822(3) yes
P(2) C(51) 1.806(3) yes
O(01) C(01) 1.147(4) yes
O(02) C(02) 1.150(4) yes
N(1) N(2) 1.360(3) yes
N(1) C(11) 1.343(3) yes
N(2) C(13) 1.347(3) yes
C(1) C(2) 1.215(3) yes
C(11) C(12) 1.388(4) yes
C(11) C(14) 1.502(3) yes
C(12) C(13) 1.391(4) yes
C(13) C(15) 1.496(4) yes
C(21) C(22) 1.390(4) yes
C(21) C(26) 1.383(4) yes
C(22) C(23) 1.382(5) yes
C(23) C(24) 1.369(5) yes
C(24) C(25) 1.378(5) yes
C(25) C(26) 1.382(5) yes
C(31) C(32) 1.395(4) yes
C(31) C(36) 1.391(4) yes
C(32) C(33) 1.387(4) yes
C(33) C(34) 1.376(5) yes
C(34) C(35) 1.369(5) yes
C(35) C(36) 1.396(4) yes
C(41) C(42) 1.400(4) yes
C(41) C(46) 1.387(4) yes
C(42) C(43) 1.377(5) yes
C(43) C(44) 1.361(5) yes
C(44) C(45) 1.372(6) yes
C(45) C(46) 1.394(4) yes
C(51) C(52) 1.399(4) yes
C(51) C(56) 1.391(5) yes
C(52) C(53) 1.392(4) yes
C(53) C(54) 1.362(7) yes
C(54) C(55) 1.385(6) yes
C(55) C(56) 1.393(4) yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
O(01) C(52) 3.352(4) 2_645
O(01) C(23) 3.363(5) 2_545
O(01) C(33) 3.463(4) 3_565
O(01) C(34) 3.506(4) 3_565
O(01) C(53) 3.573(5) 2_645
O(01) C(55) 3.583(4) 1_455
O(02) O(02) 2.950(5) 3_666
O(02) C(02) 3.214(4) 3_666
O(02) C(2) 3.253(4) 3_666
N(1) C(44) 3.335(4) 4_564
N(1) C(43) 3.478(4) 4_564
N(2) C(35) 3.432(4) 4_565
N(2) C(44) 3.486(4) 4_564
C(11) C(44) 3.546(5) 4_564
C(22) C(54) 3.557(5) 1_455
C(25) C(25) 3.510(8) 3_575
C(26) C(53) 3.451(5) 4_464
C(26) C(54) 3.479(4) 4_464
