#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:04:53 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178767 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/21/4102100.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_4102100
loop_
_publ_author_name
'Satoshi Takamizawa'
'Ei-ichi Nataka'
'Takamasa Akatsuka'
'Ryosuke Miyake'
'Yoshiki Kakizaki'
'Hirotoshi Takeuchi'
'Goro Maruta'
'Sadamu Takeda'
_publ_section_title
;
 Crystal Transformation and Host Molecular Motions in CO2 Adsorption
 Process of a Metal Benzoate Pyrazine (MII= Rh, Cu)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3783
_journal_page_last               3792
_journal_paper_doi               10.1021/ja9091598
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C32 H24 N2 O8 Rh2'
_chemical_formula_weight         770.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 127.541(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.8096(18)
_cell_length_b                   9.5907(10)
_cell_length_c                   12.3463(13)
_cell_measurement_temperature    298
_cell_volume                     1672.1(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6092
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_T_max  0.9796
_exptl_absorpt_correction_T_min  0.7463
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS; sheldrick, 1996
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2196
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0390
_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)+(0.0519P)²+1.6131P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                1872
_reflns_number_total             2196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9091598_si_001_01.cif
_cod_data_source_block           60725a1_1a_298K
_cod_database_code               4102100
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1711(3) 0.5000 0.0714(5) 0.0391(10) Uani 1 2 d SU . .
C2 C 0.2714(4) 0.5000 0.1218(5) 0.0413(10) Uani 1 2 d SU . .
C3 C 0.3181(3) 0.3757(4) 0.1446(5) 0.0551(9) Uani 1 1 d U . .
H3 H 0.2860 0.2915 0.1236 0.066 Uiso 1 1 calc R . .
C4 C 0.4131(3) 0.3765(5) 0.1990(6) 0.0687(11) Uani 1 1 d U . .
H4 H 0.4449 0.2929 0.2152 0.082 Uiso 1 1 calc R . .
C5 C 0.4598(5) 0.5000 0.2285(8) 0.0706(16) Uani 1 2 d SU . .
H5 H 0.5242 0.5000 0.2694 0.085 Uiso 1 2 calc SR . .
C6 C 0.0710(4) 0.5000 0.2581(6) 0.0488(12) Uani 1 2 d SU . .
C7 C 0.1053(5) 0.5000 0.4015(7) 0.0634(14) Uani 1 2 d SU . .
C8 C 0.1221(5) 0.3776(6) 0.4687(7) 0.0977(17) Uani 1 1 d U . .
H8 H 0.1152 0.2937 0.4258 0.117 Uiso 1 1 calc R . .
C9 C 0.1498(6) 0.3767(8) 0.6025(8) 0.118(2) Uani 1 1 d U . .
H9 H 0.1623 0.2935 0.6495 0.142 Uiso 1 1 calc R . .
C10 C 0.1576(8) 0.5000 0.6603(11) 0.113(3) Uani 1 2 d SU . .
H10 H 0.1690 0.5000 0.7445 0.135 Uiso 1 2 calc SR . .
C11 C 0.0791(3) 0.0720(3) 0.0847(4) 0.0446(8) Uani 1 1 d U . .
H11 H 0.1359 0.1190 0.1456 0.053 Uiso 1 1 calc R . .
N1 N 0.0000 0.1459(4) 0.0000 0.0432(10) Uani 1 2 d S . .
O1 O 0.13286(19) 0.3828(2) 0.0538(3) 0.0477(6) Uani 1 1 d . . .
O2 O 0.0563(2) 0.3830(2) 0.2008(3) 0.0505(6) Uani 1 1 d . . .
Rh1 Rh 0.0000 0.37530(3) 0.0000 0.03635(15) Uani 1 2 d S . .
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
_geom_angle_publ_flag
O1 C1 O1 125.8(5) . 6_565 ?
O1 C1 C2 117.1(2) . . ?
O1 C1 C2 117.1(2) 6_565 . ?
C3 C2 C3 119.3(5) 6_565 . ?
C3 C2 C1 120.3(3) 6_565 . ?
C3 C2 C1 120.3(3) . . ?
C2 C3 C4 119.9(4) . . ?
C5 C4 C3 119.9(5) . . ?
C4 C5 C4 120.8(7) . 6_565 ?
O2 C6 O2 124.8(5) . 6_565 ?
O2 C6 C7 117.6(3) . . ?
O2 C6 C7 117.6(3) 6_565 . ?
C8 C7 C8 119.2(8) 6_565 . ?
C8 C7 C6 120.4(4) 6_565 . ?
C8 C7 C6 120.4(4) . . ?
C7 C8 C9 120.7(6) . . ?
C10 C9 C8 117.8(7) . . ?
C9 C10 C9 123.3(11) . 6_565 ?
N1 C11 C11 122.0(2) . 6 ?
C11 N1 C11 116.0(4) 2 . ?
C11 N1 Rh1 122.0(2) 2 . ?
C11 N1 Rh1 122.0(2) . . ?
C1 O1 Rh1 119.1(3) . . ?
C6 O2 Rh1 119.6(3) . . ?
O2 Rh1 O2 175.86(13) . 2 ?
O2 Rh1 O1 90.48(12) . 2 ?
O2 Rh1 O1 89.37(12) 2 2 ?
O2 Rh1 O1 89.37(12) . . ?
O2 Rh1 O1 90.48(12) 2 . ?
O1 Rh1 O1 175.96(12) 2 . ?
O2 Rh1 N1 92.07(6) . . ?
O2 Rh1 N1 92.07(6) 2 . ?
O1 Rh1 N1 92.02(6) 2 . ?
O1 Rh1 N1 92.02(6) . . ?
O2 Rh1 Rh1 87.93(6) . 5_565 ?
O2 Rh1 Rh1 87.93(6) 2 5_565 ?
O1 Rh1 Rh1 87.98(6) 2 5_565 ?
O1 Rh1 Rh1 87.98(6) . 5_565 ?
N1 Rh1 Rh1 180.0 . 5_565 ?
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
C1 O1 1.263(3) . ?
C1 O1 1.263(3) 6_565 ?
C1 C2 1.490(7) . ?
C2 C3 1.381(4) 6_565 ?
C2 C3 1.381(4) . ?
C3 C4 1.389(6) . ?
C4 C5 1.362(6) . ?
C5 C4 1.362(6) 6_565 ?
C6 O2 1.267(4) . ?
C6 O2 1.267(4) 6_565 ?
C6 C7 1.480(9) . ?
C7 C8 1.362(6) 6_565 ?
C7 C8 1.362(6) . ?
C8 C9 1.407(10) . ?
C9 C10 1.344(8) . ?
C10 C9 1.344(8) 6_565 ?
C11 N1 1.336(4) . ?
C11 C11 1.381(6) 6 ?
N1 C11 1.336(4) 2 ?
N1 Rh1 2.201(3) . ?
O1 Rh1 2.032(3) . ?
O2 Rh1 2.031(3) . ?
Rh1 O2 2.031(3) 2 ?
Rh1 O1 2.032(3) 2 ?
Rh1 Rh1 2.3919(7) 5_565 ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -179.4(4) . . . 6_565 ?
O1 C1 C2 C3 -1.3(7) 6_565 . . 6_565 ?
O1 C1 C2 C3 1.3(7) . . . . ?
O1 C1 C2 C3 179.4(4) 6_565 . . . ?
C3 C2 C3 C4 4.4(8) 6_565 . . . ?
C1 C2 C3 C4 -176.3(4) . . . . ?
C2 C3 C4 C5 -0.6(8) . . . . ?
C3 C4 C5 C4 -3.4(11) . . . 6_565 ?
O2 C6 C7 C8 -179.8(6) . . . 6_565 ?
O2 C6 C7 C8 -1.5(9) 6_565 . . 6_565 ?
O2 C6 C7 C8 1.5(9) . . . . ?
O2 C6 C7 C8 179.8(6) 6_565 . . . ?
C8 C7 C8 C9 4.7(13) 6_565 . . . ?
C6 C7 C8 C9 -176.6(7) . . . . ?
C7 C8 C9 C10 1.0(13) . . . . ?
C8 C9 C10 C9 -7.0(18) . . . 6_565 ?
C11 C11 N1 C11 0.0 6 . . 2 ?
C11 C11 N1 Rh1 180.0 6 . . . ?
O1 C1 O1 Rh1 -2.8(7) 6_565 . . . ?
C2 C1 O1 Rh1 175.1(3) . . . . ?
O2 C6 O2 Rh1 -2.8(8) 6_565 . . . ?
C7 C6 O2 Rh1 175.5(4) . . . . ?
C6 O2 Rh1 O2 1.3(4) . . . 2 ?
C6 O2 Rh1 O1 -86.7(4) . . . 2 ?
C6 O2 Rh1 O1 89.3(4) . . . . ?
C6 O2 Rh1 N1 -178.7(4) . . . . ?
C6 O2 Rh1 Rh1 1.3(4) . . . 5_565 ?
C1 O1 Rh1 O2 -86.7(3) . . . . ?
C1 O1 Rh1 O2 89.2(3) . . . 2 ?
C1 O1 Rh1 O1 1.3(3) . . . 2 ?
C1 O1 Rh1 N1 -178.7(3) . . . . ?
C1 O1 Rh1 Rh1 1.3(3) . . . 5_565 ?
C11 N1 Rh1 O2 122.6(2) 2 . . . ?
C11 N1 Rh1 O2 -57.4(2) . . . . ?
C11 N1 Rh1 O2 -57.4(2) 2 . . 2 ?
C11 N1 Rh1 O2 122.6(2) . . . 2 ?
C11 N1 Rh1 O1 32.0(2) 2 . . 2 ?
C11 N1 Rh1 O1 -148.0(2) . . . 2 ?
C11 N1 Rh1 O1 -148.0(2) 2 . . . ?
C11 N1 Rh1 O1 32.0(2) . . . . ?
C11 N1 Rh1 Rh1 0(12) 2 . . 5_565 ?
C11 N1 Rh1 Rh1 0(24) . . . 5_565 ?
