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#$Date: 2019-11-03 14:02:12 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221595 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/85/4128513.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_4128513
loop_
_publ_author_name
'Carné-Sánchez, Arnau'
'Albalad, Jorge'
'Grancha, Thais'
'Imaz, Inhar'
'Juanhuix, Judith'
'Larpent, Patrick'
'Furukawa, Shuhei'
'Maspoch, Daniel'
_publ_section_title
;
 Postsynthetic Covalent and Coordination Functionalization of
 Rhodium(II)-Based Metal-Organic Polyhedra.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4094
_journal_page_last               4102
_journal_paper_doi               10.1021/jacs.8b13593
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C192 H96 O120 Rh24, O'
_chemical_formula_sum            'C192 H96 O121 Rh24'
_chemical_formula_weight         6808.53
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.480(4)
_cell_length_b                   27.480(4)
_cell_length_c                   27.480(4)
_cell_measurement_reflns_used    6439
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40
_cell_measurement_theta_min      1
_cell_volume                     20752(5)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'PILATUS DECTRIS 6M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.862
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28846
_diffrn_reflns_point_group_measured_fraction_full 0.862
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        24.391
_diffrn_reflns_theta_max         24.391
_diffrn_reflns_theta_min         2.096
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.455
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_description       octahedra
_exptl_crystal_F_000             7342
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.056
_refine_diff_density_min         -1.533
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.700
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         946
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.694
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0989
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3209
_refine_ls_wR_factor_ref         0.3305
_reflns_Friedel_coverage         0.000
_reflns_number_gt                886
_reflns_number_total             946
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b13593_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        20751.5
_cod_original_formula_sum        'C192 H96 O120 Rh24, O'
_cod_database_code               4128513
_shelx_shelxl_version_number     2018/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z+1/2, x+1/2, y+1/2'
'z+1/2, x+1/2, -y+1/2'
'z+1/2, -x+1/2, y+1/2'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z+1/2, x+1/2'
'-y+1/2, z+1/2, x+1/2'
'y+1/2, z+1/2, -x+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'z+1/2, y+1/2, x+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Rh1 Rh 0.500000 0.22693(5) 0.77307(5) 0.1078(13) Uani 1 4 d S T P
Rh2 Rh 0.500000 0.28873(6) 0.71127(6) 0.1099(13) Uani 1 4 d S T P
O003 O 0.4482(4) 0.2501(4) 0.6763(3) 0.120(3) Uani 1 1 d . . .
O004 O 0.4477(5) 0.1926(4) 0.7345(4) 0.133(3) Uani 1 1 d . . .
O005 O 0.500000 0.500000 0.500000 0.080(11) Uani 1 48 d S T P
O006 O 0.500000 0.1697(5) 0.8303(5) 0.161(9) Uani 1 4 d S T P
O007 O 0.500000 0.3474(6) 0.6526(6) 0.175(9) Uani 1 4 d S T P
C5 C 0.4331(5) 0.2139(5) 0.6949(5) 0.106(4) Uani 1 1 d . . .
C1 C 0.3689(4) 0.2104(7) 0.6311(4) 0.105(5) Uani 1 2 d S T P
H1 H 0.379274 0.240863 0.620726 0.126 Uiso 1 2 calc R U P
C2 C 0.3909(6) 0.1859(6) 0.6699(6) 0.137(5) Uani 1 1 d . . .
C4 C 0.3405(7) 0.1171(9) 0.6595(7) 0.149(7) Uani 1 2 d S TU P
H4 H 0.333322 0.084787 0.666679 0.179 Uiso 1 2 calc R U P
C3 C 0.3762(7) 0.1419(6) 0.6844(6) 0.146(6) Uani 1 1 d . U .
H3 H 0.390404 0.127802 0.711652 0.176 Uiso 1 1 calc R 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
O004 Rh1 O004 175.4(6) . 19_666
O004 Rh1 O004 89.0(7) . 66_566
O004 Rh1 O004 90.8(7) 19_666 66_566
O004 Rh1 O004 90.8(7) . 52_655
O004 Rh1 O004 89.0(7) 19_666 52_655
O004 Rh1 O004 175.4(6) 66_566 52_655
O004 Rh1 O006 92.3(3) . .
O004 Rh1 O006 92.3(3) 19_666 .
O004 Rh1 O006 92.3(3) 66_566 .
O004 Rh1 O006 92.3(3) 52_655 .
O004 Rh1 Rh2 87.7(3) . .
O004 Rh1 Rh2 87.7(3) 19_666 .
O004 Rh1 Rh2 87.7(3) 66_566 .
O004 Rh1 Rh2 87.7(3) 52_655 .
O006 Rh1 Rh2 180.00(10) . .
O003 Rh2 O003 90.2(5) 52_655 19_666
O003 Rh2 O003 176.0(5) 52_655 66_566
O003 Rh2 O003 89.7(5) 19_666 66_566
O003 Rh2 O003 89.7(5) 52_655 .
O003 Rh2 O003 175.9(5) 19_666 .
O003 Rh2 O003 90.2(5) 66_566 .
O003 Rh2 O007 92.0(3) 52_655 .
O003 Rh2 O007 92.0(3) 19_666 .
O003 Rh2 O007 92.0(3) 66_566 .
O003 Rh2 O007 92.0(3) . .
O003 Rh2 Rh1 88.0(3) 52_655 .
O003 Rh2 Rh1 88.0(3) 19_666 .
O003 Rh2 Rh1 88.0(3) 66_566 .
O003 Rh2 Rh1 88.0(3) . .
O007 Rh2 Rh1 180.0(6) . .
C5 O003 Rh2 118.7(9) . .
C5 O004 Rh1 116.7(8) . .
O003 C5 O004 128.7(13) . .
O003 C5 C2 119.0(12) . .
O004 C5 C2 112.2(11) . .
C2 C1 C2 115.4(17) 70_656 .
C2 C1 H1 122.3 70_656 .
C2 C1 H1 122.3 . .
C3 C2 C1 122.1(14) . .
C3 C2 C5 123.0(13) . .
C1 C2 C5 115.0(12) . .
C3 C4 C3 117.5(19) 70_656 .
C3 C4 H4 121.3 70_656 .
C3 C4 H4 121.3 . .
C2 C3 C4 121.2(15) . .
C2 C3 H3 119.4 . .
C4 C3 H3 119.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 O004 2.020(11) .
Rh1 O004 2.020(11) 19_666
Rh1 O004 2.020(11) 66_566
Rh1 O004 2.020(11) 52_655
Rh1 O006 2.23(2) .
Rh1 Rh2 2.401(3) .
Rh2 O003 2.019(11) 52_655
Rh2 O003 2.019(11) 19_666
Rh2 O003 2.019(11) 66_566
Rh2 O003 2.019(11) .
Rh2 O007 2.28(2) .
O003 C5 1.193(15) .
O004 C5 1.300(17) .
C5 C2 1.55(2) .
C1 C2 1.399(17) 70_656
C1 C2 1.399(17) .
C1 H1 0.9300 .
C2 C3 1.33(2) .
C4 C3 1.378(19) 70_656
C4 C3 1.378(19) .
C4 H4 0.9300 .
C3 H3 0.9300 .
