#------------------------------------------------------------------------------
#$Date: 2020-11-06 12:59:22 +0100 (vie 06 de nov de 2020) $
#$Revision: 258796 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/52/7705218.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_7705218
loop_
_publ_author_name
'Kataoka, Yusuke'
'Kohara, Yoshihiro'
'Yano, Natsumi'
'Kawamoto, Tatsuya'
_publ_section_title
;
 Unique vapochromism of a paddlewheel-type dirhodium complex accompanied
 by dynamic structural and phase transitions.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14373
_journal_page_last               14377
_journal_paper_doi               10.1039/d0dt02672g
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C24 H44 O8 Rh2'
_chemical_formula_weight         666.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-07-23 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                81.037(4)
_cell_angle_beta                 84.396(4)
_cell_angle_gamma                77.057(4)
_cell_formula_units_Z            1
_cell_length_a                   5.2013(3)
_cell_length_b                   8.4703(4)
_cell_length_c                   16.6563(7)
_cell_measurement_reflns_used    5260
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.34
_cell_measurement_theta_min      2.62
_cell_volume                     704.94(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4243
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        24.244
_diffrn_reflns_theta_max         24.244
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Chip
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.1200
_exptl_crystal_size_mid          0.0400
_exptl_crystal_size_min          0.0100
_refine_diff_density_max         0.484
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0232
_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)+(0.0527P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2069
_reflns_number_total             2184
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02672g2.cif
_cod_data_source_block           '[Rh2(HC)4]n'
_cod_depositor_comments
'Adding full bibliography for 7705218--7705220.cif.'
_cod_database_code               7705218
_shelx_shelxl_version_number     2014/7
_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'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.28730(4) 0.00793(2) 0.03393(2) 0.01762(13) Uani 1 1 d . . . . .
O1 O 0.1549(4) -0.0224(2) -0.07306(13) 0.0200(5) Uani 1 1 d . . . . .
O2 O 0.4443(4) 0.0383(3) 0.13696(13) 0.0234(5) Uani 1 1 d . . . . .
O3 O 0.2142(4) 0.2522(2) -0.00274(13) 0.0232(5) Uani 1 1 d . . . . .
O4 O 0.3833(4) -0.2387(2) 0.06885(13) 0.0228(5) Uani 1 1 d . . . . .
C1 C 0.3132(6) -0.0365(3) -0.13574(17) 0.0193(6) Uani 1 1 d . . . . .
C2 C 0.1950(6) -0.0464(4) -0.21283(18) 0.0267(7) Uani 1 1 d . . . . .
H2A H 0.1043 0.0627 -0.2345 0.032 Uiso 1 1 calc R U . . .
H2B H 0.0633 -0.1130 -0.1997 0.032 Uiso 1 1 calc R U . . .
C3 C 0.3886(7) -0.1160(4) -0.2785(2) 0.0341(8) Uani 1 1 d . . . . .
H3A H 0.4837 -0.2239 -0.2568 0.041 Uiso 1 1 calc R U . . .
H3B H 0.5164 -0.0472 -0.2938 0.041 Uiso 1 1 calc R U . . .
C4 C 0.2558(7) -0.1285(4) -0.3539(2) 0.0366(8) Uani 1 1 d . . . . .
H4A H 0.1170 -0.1888 -0.3374 0.044 Uiso 1 1 calc R U . . .
H4B H 0.1730 -0.0191 -0.3777 0.044 Uiso 1 1 calc R U . . .
C5 C 0.4390(9) -0.2104(6) -0.4182(2) 0.0575(11) Uani 1 1 d . . . . .
H5A H 0.5807 -0.1520 -0.4336 0.069 Uiso 1 1 calc R U . . .
H5B H 0.5178 -0.3210 -0.3949 0.069 Uiso 1 1 calc R U . . .
C6 C 0.3071(10) -0.2180(6) -0.4937(3) 0.0694(14) Uani 1 1 d . . . . .
H6A H 0.4353 -0.2715 -0.5317 0.083 Uiso 1 1 calc R U . . .
H6B H 0.1695 -0.2782 -0.4794 0.083 Uiso 1 1 calc R U . . .
H6C H 0.2324 -0.1091 -0.5182 0.083 Uiso 1 1 calc R U . . .
C7 C 0.3856(6) 0.3145(3) -0.04817(18) 0.0227(6) Uani 1 1 d . . . . .
C8 C 0.2995(6) 0.4912(3) -0.0826(2) 0.0276(7) Uani 1 1 d . . . . .
H8A H 0.4495 0.5311 -0.1108 0.033 Uiso 1 1 calc R U . . .
H8B H 0.2320 0.5554 -0.0388 0.033 Uiso 1 1 calc R U . . .
C9 C 0.0834(6) 0.5103(4) -0.1421(2) 0.0310(7) Uani 1 1 d . . . . .
H9A H -0.0555 0.4576 -0.1152 0.037 Uiso 1 1 calc R U . . .
H9B H 0.0066 0.6257 -0.1559 0.037 Uiso 1 1 calc R U . . .
C10 C 0.1838(7) 0.4379(4) -0.2198(2) 0.0379(8) Uani 1 1 d . . . . .
H10A H 0.3109 0.4973 -0.2494 0.046 Uiso 1 1 calc R U . . .
H10B H 0.2746 0.3250 -0.2060 0.046 Uiso 1 1 calc R U . . .
C11 C -0.0352(9) 0.4442(5) -0.2743(2) 0.0534(11) Uani 1 1 d . . . . .
H11A H -0.1364 0.5557 -0.2836 0.064 Uiso 1 1 calc R U . . .
H11B H -0.1531 0.3764 -0.2464 0.064 Uiso 1 1 calc R U . . .
C12 C 0.0639(12) 0.3866(6) -0.3565(3) 0.0748(15) Uani 1 1 d . . . . .
H12A H -0.0841 0.3936 -0.3881 0.090 Uiso 1 1 calc R U . . .
H12B H 0.1774 0.4548 -0.3852 0.090 Uiso 1 1 calc R U . . .
H12C H 0.1607 0.2754 -0.3479 0.090 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'
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
O3 Rh1 O4 176.70(7) . . ?
O3 Rh1 O1 88.92(8) . . ?
O4 Rh1 O1 91.64(8) . . ?
O3 Rh1 O2 90.73(9) . . ?
O4 Rh1 O2 88.49(8) . . ?
O1 Rh1 O2 176.13(7) . . ?
O3 Rh1 O1 90.42(8) . 2 ?
O4 Rh1 O1 92.88(8) . 2 ?
O1 Rh1 O1 80.24(9) . 2 ?
O2 Rh1 O1 103.62(8) . 2 ?
O3 Rh1 Rh1 88.01(6) . 2_655 ?
O4 Rh1 Rh1 88.76(6) . 2_655 ?
O1 Rh1 Rh1 87.74(6) . 2_655 ?
O2 Rh1 Rh1 88.40(6) . 2_655 ?
O1 Rh1 Rh1 167.90(6) 2 2_655 ?
C1 O1 Rh1 120.02(18) . . ?
C1 O1 Rh1 140.16(19) . 2 ?
Rh1 O1 Rh1 99.76(9) . 2 ?
C1 O2 Rh1 119.52(19) 2_655 . ?
C7 O3 Rh1 119.59(19) . . ?
C7 O4 Rh1 117.87(19) 2_655 . ?
O2 C1 O1 124.3(3) 2_655 . ?
O2 C1 C2 119.4(3) 2_655 . ?
O1 C1 C2 116.3(3) . . ?
C1 C2 C3 115.4(3) . . ?
C1 C2 H2A 108.4 . . ?
C3 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
C3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
C2 C3 C4 112.9(3) . . ?
C2 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C5 C4 C3 114.6(3) . . ?
C5 C4 H4A 108.6 . . ?
C3 C4 H4A 108.6 . . ?
C5 C4 H4B 108.6 . . ?
C3 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
C6 C5 C4 114.2(4) . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5B 108.7 . . ?
C4 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O3 C7 O4 125.5(3) . 2_655 ?
O3 C7 C8 115.9(3) . . ?
O4 C7 C8 118.5(3) 2_655 . ?
C7 C8 C9 109.8(2) . . ?
C7 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
C7 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C10 C9 C8 113.4(3) . . ?
C10 C9 H9A 108.9 . . ?
C8 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
C8 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C11 C10 C9 112.7(3) . . ?
C11 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
C10 C11 C12 113.6(4) . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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 O3 2.024(2) . ?
Rh1 O4 2.040(2) . ?
Rh1 O1 2.044(2) . ?
Rh1 O2 2.046(2) . ?
Rh1 O1 2.310(2) 2 ?
Rh1 Rh1 2.3700(4) 2_655 ?
O1 C1 1.268(4) . ?
O1 Rh1 2.310(2) 2 ?
O2 C1 1.256(4) 2_655 ?
O3 C7 1.265(4) . ?
O4 C7 1.272(4) 2_655 ?
C1 O2 1.256(4) 2_655 ?
C1 C2 1.498(4) . ?
C2 C3 1.509(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.519(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.508(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.507(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 O4 1.272(4) 2_655 ?
C7 C8 1.500(4) . ?
C8 C9 1.536(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.516(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.511(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.528(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
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
Rh1 O1 C1 O2 2.3(4) . . . 2_655 ?
Rh1 O1 C1 O2 178.90(16) 2 . . 2_655 ?
Rh1 O1 C1 C2 -175.80(18) . . . . ?
Rh1 O1 C1 C2 0.8(4) 2 . . . ?
O2 C1 C2 C3 20.6(4) 2_655 . . . ?
O1 C1 C2 C3 -161.2(3) . . . . ?
C1 C2 C3 C4 177.9(3) . . . . ?
C2 C3 C4 C5 -175.1(3) . . . . ?
C3 C4 C5 C6 -178.4(3) . . . . ?
Rh1 O3 C7 O4 -6.1(4) . . . 2_655 ?
Rh1 O3 C7 C8 171.10(18) . . . . ?
O3 C7 C8 C9 -66.3(3) . . . . ?
O4 C7 C8 C9 111.1(3) 2_655 . . . ?
C7 C8 C9 C10 -69.2(3) . . . . ?
C8 C9 C10 C11 174.9(3) . . . . ?
C9 C10 C11 C12 174.6(4) . . . . ?
