#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:28:45 +0100 (vie 25 de mar de 2016) $
#$Revision: 179792 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/88/7008860.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_7008860
loop_
_publ_author_name
'Berry, John F.'
'Cotton, F. Albert'
'Huang, Penglin'
'Murillo, Carlos A.'
'Wang, Xiaoping'
_publ_section_title
;
 A hardwon dirhodium paddlewheel with guanidinate type (hpp) bridging
 ligands
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              3713
_journal_paper_doi               10.1039/b513406d
_journal_year                    2005
_chemical_formula_moiety         'C27 H47 N9 O6 Rh2, 2(C H2 Cl2)'
_chemical_formula_sum            'C29 H51 Cl4 N9 O6 Rh2'
_chemical_formula_weight         969.41
_chemical_name_common            'Rh2(hpp)(OAc)3(Hhpp)2, 2CH2Cl2'
_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                 108.844(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.952(3)
_cell_length_b                   13.2172(19)
_cell_length_c                   14.875(2)
_cell_measurement_reflns_used    7575
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     3898.5(10)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12802
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  0.9018
_exptl_absorpt_correction_T_min  0.7581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4420
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0322P)²+7.4775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                3754
_reflns_number_total             4420
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b513406d.txt
_cod_data_source_block           Three2CH2Cl2
_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_sg_symbol_H-M      C2/c
_cod_database_code               7008860
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.440172(8) 0.633459(14) 0.239818(12) 0.02703(7) Uani 1 1 d . . .
N1 N 0.44166(9) 0.48180(16) 0.22627(14) 0.0307(4) Uani 1 1 d . . .
N2 N 0.5000 0.3261(2) 0.2500 0.0349(6) Uani 1 2 d S . .
N3 N 0.32704(10) 0.64764(16) 0.22098(15) 0.0327(5) Uani 1 1 d . . .
N4 N 0.22472(11) 0.60311(18) 0.24602(17) 0.0389(5) Uani 1 1 d . . .
N5 N 0.32862(11) 0.5602(2) 0.35414(16) 0.0405(5) Uani 1 1 d . . .
H5 H 0.3686(16) 0.559(2) 0.367(2) 0.049 Uiso 1 1 d . . .
O1 O 0.44609(9) 0.79127(14) 0.24950(13) 0.0387(4) Uani 1 1 d . . .
O2 O 0.42185(8) 0.64423(13) 0.09603(12) 0.0344(4) Uani 1 1 d . . .
O3 O 0.53251(8) 0.62534(13) 0.11464(12) 0.0318(4) Uani 1 1 d . . .
C1 C 0.37827(12) 0.4271(2) 0.18958(19) 0.0368(6) Uani 1 1 d . . .
H1A H 0.3443 0.4711 0.1466 0.044 Uiso 1 1 calc R . .
H1B H 0.3623 0.4083 0.2424 0.044 Uiso 1 1 calc R . .
C2 C 0.38650(13) 0.3327(2) 0.1368(2) 0.0430(6) Uani 1 1 d . . .
H2A H 0.3437 0.2956 0.1146 0.052 Uiso 1 1 calc R . .
H2B H 0.3997 0.3510 0.0815 0.052 Uiso 1 1 calc R . .
C3 C 0.44021(14) 0.2673(2) 0.2038(2) 0.0447(6) Uani 1 1 d . . .
H3A H 0.4229 0.2380 0.2518 0.054 Uiso 1 1 calc R . .
H3B H 0.4517 0.2117 0.1682 0.054 Uiso 1 1 calc R . .
C4 C 0.5000 0.4314(3) 0.2500 0.0284(7) Uani 1 2 d S . .
C5 C 0.47090(12) 0.63632(19) 0.06481(18) 0.0318(5) Uani 1 1 d . B .
C6 C 0.45625(14) 0.6417(2) -0.04116(19) 0.0412(6) Uani 1 1 d . . .
H6A H 0.4980 0.6345 -0.0556 0.062 Uiso 0.50 1 calc PR A 1
H6B H 0.4358 0.7065 -0.0645 0.062 Uiso 0.50 1 calc PR A 1
H6C H 0.4256 0.5876 -0.0716 0.062 Uiso 0.50 1 calc PR A 1
H6D H 0.4713 0.5798 -0.0631 0.062 Uiso 0.50 1 calc PR A 2
H6E H 0.4799 0.6989 -0.0563 0.062 Uiso 0.50 1 calc PR A 2
H6F H 0.4081 0.6498 -0.0723 0.062 Uiso 0.50 1 calc PR A 2
C7 C 0.5000 0.8348(3) 0.2500 0.0407(8) Uani 1 2 d S . .
C8 C 0.5000 0.9491(3) 0.2500 0.0680(15) Uani 1 2 d S . .
H8A H 0.5437 0.9735 0.2502 0.102 Uiso 0.50 1 calc PR B .
H8B H 0.4909 0.9735 0.3061 0.102 Uiso 0.50 1 calc PR . .
H8C H 0.4654 0.9735 0.1936 0.102 Uiso 0.50 1 calc PR . .
C9A C 0.28912(14) 0.7005(3) 0.1331(2) 0.0511(8) Uani 0.55 1 d PD B 1
H9AA H 0.2914 0.6597 0.0792 0.061 Uiso 0.55 1 calc PR B 1
H9AB H 0.3120 0.7647 0.1310 0.061 Uiso 0.55 1 calc PR B 1
C10A C 0.2178(2) 0.7225(5) 0.1194(5) 0.0460(13) Uani 0.55 1 d PD B 1
H10A H 0.2149 0.7873 0.1499 0.055 Uiso 0.55 1 calc PR B 1
H10B H 0.1939 0.7300 0.0513 0.055 Uiso 0.55 1 calc PR B 1
C11A C 0.18429(16) 0.6466(3) 0.1569(3) 0.0732(13) Uani 0.55 1 d PD B 1
H11A H 0.1695 0.5922 0.1100 0.088 Uiso 0.55 1 calc PR B 1
H11B H 0.1439 0.6766 0.1654 0.088 Uiso 0.55 1 calc PR B 1
C9B C 0.28912(14) 0.7005(3) 0.1331(2) 0.0511(8) Uani 0.45 1 d PD B 2
H9BA H 0.2899 0.7733 0.1459 0.061 Uiso 0.45 1 calc PR B 2
H9BB H 0.3116 0.6895 0.0855 0.061 Uiso 0.45 1 calc PR B 2
C10B C 0.2206(3) 0.6680(7) 0.0949(5) 0.056(2) Uani 0.45 1 d PD B 2
H10C H 0.1959 0.7204 0.0508 0.067 Uiso 0.45 1 calc PR B 2
H10D H 0.2200 0.6070 0.0572 0.067 Uiso 0.45 1 calc PR B 2
C11B C 0.18429(16) 0.6466(3) 0.1569(3) 0.0732(13) Uani 0.45 1 d PD B 2
H11C H 0.1477 0.5996 0.1255 0.088 Uiso 0.45 1 calc PR B 2
H11D H 0.1638 0.7093 0.1697 0.088 Uiso 0.45 1 calc PR B 2
C12 C 0.29360(12) 0.60619(18) 0.27092(17) 0.0300(5) Uani 1 1 d . B .
C13A C 0.18981(15) 0.5559(3) 0.3043(3) 0.0711(12) Uani 0.48 1 d PD B 1
H13A H 0.1532 0.6006 0.3073 0.085 Uiso 0.48 1 calc PR B 1
H13B H 0.1694 0.4927 0.2739 0.085 Uiso 0.48 1 calc PR B 1
C13B C 0.18981(15) 0.5559(3) 0.3043(3) 0.0711(12) Uani 0.52 1 d PD B 2
H13C H 0.1522 0.5167 0.2624 0.085 Uiso 0.52 1 calc PR B 2
H13D H 0.1703 0.6097 0.3326 0.085 Uiso 0.52 1 calc PR B 2
C14A C 0.2314(3) 0.5342(7) 0.3977(7) 0.059(3) Uani 0.48 1 d PD B 1
H14A H 0.2292 0.5927 0.4372 0.070 Uiso 0.48 1 calc PR B 1
H14B H 0.2110 0.4771 0.4205 0.070 Uiso 0.48 1 calc PR B 1
C14B C 0.2281(3) 0.4896(6) 0.3802(7) 0.060(3) Uani 0.52 1 d PD B 2
H14C H 0.2097 0.4944 0.4328 0.072 Uiso 0.52 1 calc PR B 2
H14D H 0.2221 0.4197 0.3571 0.072 Uiso 0.52 1 calc PR B 2
C15A C 0.29897(16) 0.5115(4) 0.4159(3) 0.0755(13) Uani 0.48 1 d PD B 1
H15A H 0.3036 0.4381 0.4106 0.091 Uiso 0.48 1 calc PR B 1
H15B H 0.3240 0.5308 0.4815 0.091 Uiso 0.48 1 calc PR B 1
C15B C 0.29897(16) 0.5115(4) 0.4159(3) 0.0755(13) Uani 0.52 1 d PD B 2
H15C H 0.3072 0.5538 0.4726 0.091 Uiso 0.52 1 calc PR B 2
H15D H 0.3229 0.4475 0.4364 0.091 Uiso 0.52 1 calc PR B 2
C1S C 0.12384(16) 0.3194(3) 0.0961(3) 0.0578(8) Uani 1 1 d . . .
H1SA H 0.1185 0.3197 0.1592 0.069 Uiso 1 1 calc R . .
H1SB H 0.1127 0.2514 0.0694 0.069 Uiso 1 1 calc R . .
Cl1 Cl 0.06731(6) 0.40573(10) 0.02357(9) 0.0909(3) Uani 1 1 d . . .
Cl2 Cl 0.20738(5) 0.34552(10) 0.10791(11) 0.0952(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'
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'
Cl Cl 0.1484 0.1585 '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
N1 Rh1 O2 88.20(7) . . ?
N1 Rh1 O3 92.60(7) . 2_655 ?
O2 Rh1 O3 174.83(6) . 2_655 ?
N1 Rh1 O1 174.86(7) . . ?
O2 Rh1 O1 89.40(7) . . ?
O3 Rh1 O1 89.39(7) 2_655 . ?
N1 Rh1 N3 96.74(7) . . ?
O2 Rh1 N3 91.65(7) . . ?
O3 Rh1 N3 93.32(7) 2_655 . ?
O1 Rh1 N3 87.88(7) . . ?
N1 Rh1 Rh1 87.92(5) . 2_655 ?
O2 Rh1 Rh1 88.17(5) . 2_655 ?
O3 Rh1 Rh1 86.76(5) 2_655 2_655 ?
O1 Rh1 Rh1 87.45(5) . 2_655 ?
N3 Rh1 Rh1 175.33(5) . 2_655 ?
C4 N1 C1 119.9(2) . . ?
C4 N1 Rh1 120.78(18) . . ?
C1 N1 Rh1 119.35(15) . . ?
C4 N2 C3 122.51(16) . . ?
C4 N2 C3 122.51(16) . 2_655 ?
C3 N2 C3 115.0(3) . 2_655 ?
C12 N3 C9A 118.3(2) . . ?
C12 N3 Rh1 128.44(17) . . ?
C9A N3 Rh1 112.75(15) . . ?
C12 N4 C11A 119.4(2) . . ?
C12 N4 C13A 123.0(2) . . ?
C11A N4 C13A 117.6(2) . . ?
C12 N5 C15A 124.8(2) . . ?
C7 O1 Rh1 119.12(19) . . ?
C5 O2 Rh1 118.53(16) . . ?
C5 O3 Rh1 119.52(15) . 2_655 ?
N1 C1 C2 111.2(2) . . ?
C3 C2 C1 108.4(2) . . ?
N2 C3 C2 110.7(2) . . ?
N1 C4 N1 120.2(3) . 2_655 ?
N1 C4 N2 119.91(15) . . ?
N1 C4 N2 119.91(15) 2_655 . ?
O2 C5 O3 126.1(2) . . ?
O2 C5 C6 117.8(2) . . ?
O3 C5 C6 116.1(2) . . ?
O1 C7 O1 125.9(4) 2_655 . ?
O1 C7 C8 117.04(18) 2_655 . ?
O1 C7 C8 117.04(18) . . ?
N3 C9A C10A 116.8(3) . . ?
C11A C10A C9A 114.2(4) . . ?
C10A C11A N4 114.8(3) . . ?
N3 C12 N5 118.5(2) . . ?
N3 C12 N4 125.1(2) . . ?
N5 C12 N4 116.4(2) . . ?
C14A C13A N4 114.1(4) . . ?
C15A C14A C13A 120.2(8) . . ?
C14A C15A N5 114.1(4) . . ?
Cl2 C1S Cl1 113.17(19) . . ?
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 N1 2.016(2) . ?
Rh1 O2 2.0523(18) . ?
Rh1 O3 2.0557(17) 2_655 ?
Rh1 O1 2.0917(19) . ?
Rh1 N3 2.303(2) . ?
Rh1 Rh1 2.4262(5) 2_655 ?
N1 C4 1.335(3) . ?
N1 C1 1.455(3) . ?
N2 C4 1.392(5) . ?
N2 C3 1.445(3) . ?
N2 C3 1.445(3) 2_655 ?
N3 C12 1.296(3) . ?
N3 C9A 1.469(3) . ?
N4 C12 1.370(3) . ?
N4 C11A 1.442(4) . ?
N4 C13A 1.445(4) . ?
N5 C12 1.361(3) . ?
N5 C15A 1.419(4) . ?
O1 C7 1.266(2) . ?
O2 C5 1.261(3) . ?
O3 C5 1.272(3) . ?
O3 Rh1 2.0557(17) 2_655 ?
C1 C2 1.513(4) . ?
C2 C3 1.510(4) . ?
C4 N1 1.336(3) 2_655 ?
C5 C6 1.507(3) . ?
C7 O1 1.265(2) 2_655 ?
C7 C8 1.510(6) . ?
C9A C10A 1.471(5) . ?
C10A C11A 1.436(6) . ?
C13A C14A 1.411(8) . ?
C14A C15A 1.386(7) . ?
C1S Cl2 1.736(3) . ?
C1S Cl1 1.744(4) . ?
