#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:10:51 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180493 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/62/7216272.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_7216272
loop_
_publ_author_name
'Takamizawa, Satoshi'
'Nakata, Ei-ichi'
'Saito, Teruo'
'Kojima, Kenichi'
_publ_section_title
;
 Structural determination of physisorbed sites for CO2 and Ar gases inside
 an organometallic framework
;
_journal_issue                   72
_journal_name_full               CrystEngComm
_journal_page_first              411
_journal_paper_doi               10.1039/b312553j
_journal_volume                  5
_journal_year                    2003
_chemical_formula_sum            'C32.77 H24 N2 O9.54 Rh2'
_chemical_formula_weight         804.08
_chemical_name_common            'Rhodium(II) benzoate pyrazine'
_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-97
_cell_angle_alpha                71.270(5)
_cell_angle_beta                 66.062(4)
_cell_angle_gamma                63.155(4)
_cell_formula_units_Z            1
_cell_length_a                   9.572(2)
_cell_length_b                   10.424(2)
_cell_length_c                   10.977(2)
_cell_measurement_temperature    298
_cell_volume                     880.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      298
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0977
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3305
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  0.9614
_exptl_absorpt_correction_T_min  0.7689
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             401
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         1830
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0694
_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)+(0.1100P)²+4.4565P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2009
_refine_ls_wR_factor_ref         0.2197
_reflns_number_gt                1208
_reflns_number_total             1830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b312553j.txt
_cod_data_source_block           306131
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7216272
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.539(2) 0.1368(19) 0.2502(19) 0.050(2) Uani 1 1 d U
C2 C 0.5634(18) 0.2106(17) 0.1091(15) 0.061(3) Uani 1 1 d DU
C3 C 0.4750(17) 0.2085(16) 0.0361(15) 0.069(3) Uani 1 1 d DU
H3 H 0.4004 0.1616 0.0771 0.082 Uiso 1 1 calc R
C4 C 0.4989(19) 0.2770(18) -0.0991(16) 0.075(3) Uani 1 1 d DU
H4 H 0.4397 0.2760 -0.1480 0.090 Uiso 1 1 calc R
C5 C 0.611(2) 0.347(2) -0.1607(16) 0.079(3) Uani 1 1 d DU
H5 H 0.6283 0.3908 -0.2511 0.095 Uiso 1 1 calc R
C6 C 0.697(2) 0.351(2) -0.0873(16) 0.075(3) Uani 1 1 d DU
H6 H 0.7686 0.4013 -0.1271 0.090 Uiso 1 1 calc R
C7 C 0.6771(19) 0.2785(18) 0.0470(15) 0.069(3) Uani 1 1 d DU
H7 H 0.7397 0.2760 0.0947 0.082 Uiso 1 1 calc R
C8 C 0.3318(18) 0.2520(17) 0.5759(17) 0.042(3) Uani 1 1 d U
C9 C 0.2319(14) 0.4027(14) 0.6154(15) 0.045(2) Uani 1 1 d DU
C10 C 0.0638(14) 0.4625(14) 0.6408(14) 0.051(3) Uani 1 1 d DU
H10 H 0.0108 0.4111 0.6327 0.062 Uiso 1 1 calc R
C11 C -0.0258(15) 0.5980(14) 0.6779(16) 0.058(3) Uani 1 1 d DU
H11 H -0.1391 0.6390 0.6938 0.069 Uiso 1 1 calc R
C12 C 0.0529(15) 0.6729(15) 0.6916(18) 0.059(3) Uani 1 1 d DU
H12 H -0.0077 0.7632 0.7197 0.070 Uiso 1 1 calc R
C13 C 0.2204(15) 0.6143(15) 0.6637(18) 0.054(3) Uani 1 1 d DU
H13 H 0.2738 0.6668 0.6694 0.065 Uiso 1 1 calc R
C14 C 0.3101(15) 0.4787(14) 0.6276(17) 0.049(3) Uani 1 1 d DU
H14 H 0.4234 0.4382 0.6114 0.059 Uiso 1 1 calc R
C15 C 0.0025(17) 0.0542(16) 0.5923(16) 0.036(3) Uani 1 1 d U
H15 H 0.0005 0.0947 0.6573 0.044 Uiso 1 1 calc R
C16 C 0.1428(18) -0.0619(17) 0.4119(17) 0.037(3) Uani 1 1 d U
H16 H 0.2410 -0.1045 0.3477 0.044 Uiso 1 1 calc R
C1S C 0.0000 0.5000 0.0000 0.22(2) Uani 0.77(5) 2 d SPU
N1 N 0.1449(14) -0.0099(14) 0.5052(14) 0.035(3) Uani 1 1 d U
O1 O 0.4173(12) 0.0972(12) 0.3061(11) 0.047(2) Uani 1 1 d U
O2 O 0.6469(12) 0.1115(11) 0.3033(11) 0.044(2) Uani 1 1 d U
O3 O 0.2545(12) 0.1885(11) 0.5631(11) 0.041(2) Uani 1 1 d U
O4 O 0.5145(11) -0.2006(11) 0.4396(11) 0.039(3) Uani 1 1 d U
O1S O -0.003(5) 0.589(4) 0.012(4) 0.22(2) Uani 0.77(5) 1 d PU
Rh1 Rh 0.37726(15) -0.00617(15) 0.50248(16) 0.0349(6) Uani 1 1 d U
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'
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
O1 C1 O2 125.7(17) . .
O1 C1 C2 116.9(15) . .
O2 C1 C2 117.3(14) . .
C7 C2 C3 120.1(9) . .
C7 C2 C1 120.5(12) . .
C3 C2 C1 119.3(12) . .
C2 C3 C4 119.7(9) . .
C5 C4 C3 120.2(9) . .
C6 C5 C4 120.0(9) . .
C5 C6 C7 119.8(9) . .
C2 C7 C6 120.1(9) . .
O3 C8 O4 125.9(14) . 2_656
O3 C8 C9 117.0(13) . .
O4 C8 C9 117.1(12) 2_656 .
C14 C9 C10 119.9(8) . .
C14 C9 C8 119.6(10) . .
C10 C9 C8 120.5(10) . .
C11 C10 C9 120.1(9) . .
C10 C11 C12 119.7(9) . .
C13 C12 C11 119.9(9) . .
C12 C13 C14 120.5(9) . .
C13 C14 C9 119.8(9) . .
N1 C15 C16 121.0(14) . 2_556
N1 C16 C15 121.0(14) . 2_556
O1S C1S O1S 180(5) 2_565 .
C16 N1 C15 117.9(13) . .
C16 N1 Rh1 121.1(10) . .
C15 N1 Rh1 120.7(11) . .
C1 O1 Rh1 118.7(11) . .
C1 O2 Rh1 119.2(11) . 2_656
C8 O3 Rh1 119.8(10) . .
C8 O4 Rh1 117.8(9) 2_656 .
O3 Rh1 O4 176.3(4) . .
O3 Rh1 O2 91.3(4) . 2_656
O4 Rh1 O2 89.1(4) . 2_656
O3 Rh1 O1 89.5(4) . .
O4 Rh1 O1 90.0(4) . .
O2 Rh1 O1 176.1(4) 2_656 .
O3 Rh1 N1 90.8(4) . .
O4 Rh1 N1 92.8(4) . .
O2 Rh1 N1 93.0(5) 2_656 .
O1 Rh1 N1 90.8(5) . .
O3 Rh1 Rh1 87.6(3) . 2_656
O4 Rh1 Rh1 88.7(3) . 2_656
O2 Rh1 Rh1 88.0(3) 2_656 2_656
O1 Rh1 Rh1 88.2(3) . 2_656
N1 Rh1 Rh1 178.2(4) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.264(18) .
C1 O2 1.271(18) .
C1 C2 1.47(2) .
C2 C7 1.391(13) .
C2 C3 1.391(13) .
C3 C4 1.399(13) .
C4 C5 1.394(13) .
C5 C6 1.388(13) .
C6 C7 1.402(13) .
C8 O3 1.262(17) .
C8 O4 1.274(16) 2_656
C8 C9 1.522(19) .
C9 C14 1.375(12) .
C9 C10 1.377(12) .
C10 C11 1.375(12) .
C11 C12 1.377(12) .
C12 C13 1.370(12) .
C13 C14 1.371(12) .
C15 N1 1.322(17) .
C15 C16 1.37(2) 2_556
C16 N1 1.314(18) .
C16 C15 1.37(2) 2_556
C1S O1S 0.96(4) 2_565
C1S O1S 0.96(4) .
N1 Rh1 2.230(12) .
O1 Rh1 2.041(11) .
O2 Rh1 2.033(11) 2_656
O3 Rh1 2.005(10) .
O4 C8 1.274(16) 2_656
O4 Rh1 2.017(10) .
Rh1 O2 2.033(11) 2_656
Rh1 Rh1 2.389(2) 2_656
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 C1 C2 C7 169.4(15) . .
O2 C1 C2 C7 -14(2) . .
O1 C1 C2 C3 -13(2) . .
O2 C1 C2 C3 164.0(13) . .
C7 C2 C3 C4 -1.1(16) . .
C1 C2 C3 C4 -179.2(15) . .
C2 C3 C4 C5 0.2(16) . .
C3 C4 C5 C6 -1(3) . .
C4 C5 C6 C7 3(3) . .
C3 C2 C7 C6 3(2) . .
C1 C2 C7 C6 -179.0(17) . .
C5 C6 C7 C2 -4(3) . .
O3 C8 C9 C14 -178.4(15) . .
O4 C8 C9 C14 2(2) 2_656 .
O3 C8 C9 C10 3(2) . .
O4 C8 C9 C10 -176.7(13) 2_656 .
C14 C9 C10 C11 0.2(16) . .
C8 C9 C10 C11 179.2(15) . .
C9 C10 C11 C12 -0.9(16) . .
C10 C11 C12 C13 2(2) . .
C11 C12 C13 C14 -3(3) . .
C12 C13 C14 C9 2(3) . .
C10 C9 C14 C13 -1(2) . .
C8 C9 C14 C13 -179.7(15) . .
C15 C16 N1 C15 -2(3) 2_556 .
C15 C16 N1 Rh1 -175.1(11) 2_556 .
C16 C15 N1 C16 2(3) 2_556 .
C16 C15 N1 Rh1 175.1(11) 2_556 .
O2 C1 O1 Rh1 4(2) . .
C2 C1 O1 Rh1 180.0(11) . .
O1 C1 O2 Rh1 -3(2) . 2_656
C2 C1 O2 Rh1 -178.9(11) . 2_656
O4 C8 O3 Rh1 -4(2) 2_656 .
C9 C8 O3 Rh1 177.0(10) . .
C8 O3 Rh1 O4 -6(8) . .
C8 O3 Rh1 O2 89.3(13) . 2_656
C8 O3 Rh1 O1 -86.9(13) . .
C8 O3 Rh1 N1 -177.7(13) . .
C8 O3 Rh1 Rh1 1.4(12) . 2_656
C8 O4 Rh1 O3 9(8) 2_656 .
C8 O4 Rh1 O2 -85.7(12) 2_656 2_656
C8 O4 Rh1 O1 90.6(12) 2_656 .
C8 O4 Rh1 N1 -178.6(12) 2_656 .
C8 O4 Rh1 Rh1 2.4(11) 2_656 2_656
C1 O1 Rh1 O3 85.1(12) . .
C1 O1 Rh1 O4 -91.3(12) . .
C1 O1 Rh1 O2 -16(7) . 2_656
C1 O1 Rh1 N1 175.9(12) . .
C1 O1 Rh1 Rh1 -2.6(12) . 2_656
C16 N1 Rh1 O3 141.6(12) . .
C15 N1 Rh1 O3 -31.2(12) . .
C16 N1 Rh1 O4 -37.9(13) . .
C15 N1 Rh1 O4 149.4(12) . .
C16 N1 Rh1 O2 -127.1(12) . 2_656
C15 N1 Rh1 O2 60.2(12) . 2_656
C16 N1 Rh1 O1 52.1(13) . .
C15 N1 Rh1 O1 -120.6(12) . .
C16 N1 Rh1 Rh1 109(12) . 2_656
C15 N1 Rh1 Rh1 -64(13) . 2_656
