#------------------------------------------------------------------------------
#$Date: 2020-11-06 13:59:22 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258796 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705219.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_7705219
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            'C34 H54 N2 O8 Rh2'
_chemical_formula_weight         824.61
_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                113.792(5)
_cell_angle_beta                 99.705(4)
_cell_angle_gamma                92.156(3)
_cell_formula_units_Z            1
_cell_length_a                   8.2724(3)
_cell_length_b                   10.7362(5)
_cell_length_c                   11.2851(6)
_cell_measurement_reflns_used    5845
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.7670
_cell_measurement_theta_min      2.0600
_cell_volume                     897.75(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_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    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7716
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.452
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.573
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.184
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0428P)²+1.6420P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2971
_reflns_number_total             3153
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02672g2.cif
_cod_data_source_block           '[Rh2(HC)4(py)2]'
_cod_depositor_comments
'Adding full bibliography for 7705218--7705220.cif.'
_cod_database_code               7705219
_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 0.45107(3) 0.10384(2) 1.00077(3) 0.01776(12) Uani 1 1 d . . . . .
O2 O 0.5828(3) 0.2032(2) 1.1884(3) 0.0240(6) Uani 1 1 d . . . . .
O1 O 0.3253(3) -0.0081(2) 0.8124(3) 0.0246(6) Uani 1 1 d . . . . .
O3 O 0.6523(3) 0.1338(2) 0.9293(3) 0.0254(6) Uani 1 1 d . . . . .
O4 O 0.2566(3) 0.0610(2) 1.0721(3) 0.0250(6) Uani 1 1 d . . . . .
N1 N 0.3600(3) 0.2984(3) 1.0035(3) 0.0190(6) Uani 1 1 d . . . . .
C1 C 0.6650(4) 0.1357(4) 1.2412(4) 0.0226(8) Uani 1 1 d . . . . .
C2 C 0.7631(5) 0.2115(4) 1.3787(4) 0.0278(8) Uani 1 1 d . . . . .
H2A H 0.8814 0.2038 1.3759 0.033 Uiso 1 1 calc R U . . .
H2B H 0.7331 0.1649 1.4332 0.033 Uiso 1 1 calc R U . . .
C3 C 0.7425(5) 0.3625(4) 1.4481(4) 0.0266(8) Uani 1 1 d . . . . .
H3A H 0.7736 0.4108 1.3954 0.032 Uiso 1 1 calc R U . . .
H3B H 0.6249 0.3718 1.4529 0.032 Uiso 1 1 calc R U . . .
C4 C 0.8469(5) 0.4295(4) 1.5862(4) 0.0281(8) Uani 1 1 d . . . . .
H4A H 0.9635 0.4148 1.5817 0.034 Uiso 1 1 calc R U . . .
H4B H 0.8109 0.3845 1.6403 0.034 Uiso 1 1 calc R U . . .
C5 C 0.8356(5) 0.5824(4) 1.6539(4) 0.0302(9) Uani 1 1 d . . . . .
H5A H 0.8639 0.6263 1.5968 0.036 Uiso 1 1 calc R U . . .
H5B H 0.7203 0.5966 1.6640 0.036 Uiso 1 1 calc R U . . .
C6 C 0.9486(5) 0.6515(4) 1.7883(4) 0.0333(9) Uani 1 1 d . . . . .
H6A H 0.9360 0.7495 1.8269 0.040 Uiso 1 1 calc R U . . .
H6B H 0.9197 0.6101 1.8462 0.040 Uiso 1 1 calc R U . . .
H6C H 1.0634 0.6398 1.7790 0.040 Uiso 1 1 calc R U . . .
C7 C 0.7518(4) 0.0456(4) 0.9070(4) 0.0240(8) Uani 1 1 d . . . . .
C8 C 0.8959(4) 0.0700(4) 0.8488(4) 0.0298(9) Uani 1 1 d . . . . .
H8A H 0.9729 0.1485 0.9171 0.036 Uiso 1 1 calc R U . . .
H8B H 0.9562 -0.0118 0.8243 0.036 Uiso 1 1 calc R U . . .
C9 C 0.8442(6) 0.0989(6) 0.7290(5) 0.0499(13) Uani 1 1 d . . . . .
H9A H 0.8012 0.1890 0.7585 0.060 Uiso 1 1 calc R U . . .
H9B H 0.9446 0.1083 0.6950 0.060 Uiso 1 1 calc R U . . .
C10 C 0.7198(9) -0.0003(8) 0.6170(6) 0.089(2) Uani 1 1 d . U . . .
H10A H 0.6311 -0.0257 0.6549 0.106 Uiso 1 1 calc R U . . .
H10B H 0.6702 0.0494 0.5654 0.106 Uiso 1 1 calc R U . . .
C12 C 0.6357(9) -0.2269(7) 0.4226(8) 0.0992(13) Uani 1 1 d . U . . .
H12A H 0.6918 -0.3033 0.3712 0.119 Uiso 1 1 calc R U . . .
H12B H 0.5564 -0.2599 0.4620 0.119 Uiso 1 1 calc R U . . .
H12C H 0.5772 -0.1886 0.3644 0.119 Uiso 1 1 calc R U . . .
C13 C 0.4115(4) 0.4192(4) 1.1053(4) 0.0254(8) Uani 1 1 d . . . . .
H13 H 0.4887 0.4226 1.1795 0.031 Uiso 1 1 calc R U . . .
C14 C 0.3571(5) 0.5391(4) 1.1070(4) 0.0287(9) Uani 1 1 d . . . . .
H14 H 0.3977 0.6237 1.1807 0.034 Uiso 1 1 calc R U . . .
C15 C 0.2437(5) 0.5362(4) 1.0018(4) 0.0312(9) Uani 1 1 d . . . . .
H15 H 0.2039 0.6179 1.0015 0.037 Uiso 1 1 calc R U . . .
C16 C 0.1890(5) 0.4110(4) 0.8963(4) 0.0296(9) Uani 1 1 d . . . . .
H16 H 0.1103 0.4048 0.8218 0.036 Uiso 1 1 calc R U . . .
C17 C 0.2507(4) 0.2954(4) 0.9011(4) 0.0233(8) Uani 1 1 d . . . . .
H17 H 0.2135 0.2097 0.8280 0.028 Uiso 1 1 calc R U . . .
C11 C 0.7611(9) -0.1177(7) 0.5305(8) 0.0992(13) Uani 1 1 d . U . . .
H11A H 0.8213 -0.1622 0.5835 0.119 Uiso 1 1 calc R U . . .
H11B H 0.8419 -0.0915 0.4867 0.119 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'
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
O2 Rh1 O4 89.77(11) . . ?
O2 Rh1 O1 175.98(9) . . ?
O4 Rh1 O1 90.22(11) . . ?
O2 Rh1 O3 90.04(11) . . ?
O4 Rh1 O3 175.73(9) . . ?
O1 Rh1 O3 89.67(11) . . ?
O2 Rh1 N1 91.49(10) . . ?
O4 Rh1 N1 92.19(10) . . ?
O1 Rh1 N1 92.53(10) . . ?
O3 Rh1 N1 92.08(10) . . ?
O2 Rh1 Rh1 88.21(7) . 2_657 ?
O4 Rh1 Rh1 87.69(7) . 2_657 ?
O1 Rh1 Rh1 87.77(7) . 2_657 ?
O3 Rh1 Rh1 88.04(7) . 2_657 ?
N1 Rh1 Rh1 179.68(8) . 2_657 ?
C1 O2 Rh1 119.0(2) . . ?
C1 O1 Rh1 119.0(2) 2_657 . ?
C7 O3 Rh1 118.7(2) . . ?
C7 O4 Rh1 119.2(2) 2_657 . ?
C17 N1 C13 118.0(3) . . ?
C17 N1 Rh1 119.9(2) . . ?
C13 N1 Rh1 122.1(3) . . ?
O2 C1 O1 126.0(3) . 2_657 ?
O2 C1 C2 118.0(3) . . ?
O1 C1 C2 116.0(3) 2_657 . ?
C1 C2 C3 116.6(3) . . ?
C1 C2 H2A 108.1 . . ?
C3 C2 H2A 108.1 . . ?
C1 C2 H2B 108.1 . . ?
C3 C2 H2B 108.1 . . ?
H2A C2 H2B 107.3 . . ?
C4 C3 C2 112.4(3) . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 C5 113.0(3) . . ?
C3 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C6 C5 C4 113.2(3) . . ?
C6 C5 H5A 108.9 . . ?
C4 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?
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 126.4(3) . 2_657 ?
O3 C7 C8 116.5(3) . . ?
O4 C7 C8 117.1(3) 2_657 . ?
C9 C8 C7 113.2(3) . . ?
C9 C8 H8A 108.9 . . ?
C7 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 C8 118.7(5) . . ?
C10 C9 H9A 107.7 . . ?
C8 C9 H9A 107.7 . . ?
C10 C9 H9B 107.7 . . ?
C8 C9 H9B 107.7 . . ?
H9A C9 H9B 107.1 . . ?
C11 C10 C9 121.2(7) . . ?
C11 C10 H10A 107.0 . . ?
C9 C10 H10A 107.0 . . ?
C11 C10 H10B 107.0 . . ?
C9 C10 H10B 107.0 . . ?
H10A C10 H10B 106.8 . . ?
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 . . ?
N1 C13 C14 122.4(4) . . ?
N1 C13 H13 118.8 . . ?
C14 C13 H13 118.8 . . ?
C15 C14 C13 119.7(4) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 118.2(4) . . ?
C14 C15 H15 120.9 . . ?
C16 C15 H15 120.9 . . ?
C17 C16 C15 118.8(4) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
N1 C17 C16 122.9(3) . . ?
N1 C17 H17 118.5 . . ?
C16 C17 H17 118.5 . . ?
C10 C11 C12 122.8(7) . . ?
C10 C11 H11A 106.6 . . ?
C12 C11 H11A 106.6 . . ?
C10 C11 H11B 106.6 . . ?
C12 C11 H11B 106.6 . . ?
H11A C11 H11B 106.6 . . ?
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 O2 2.030(3) . ?
Rh1 O4 2.032(2) . ?
Rh1 O1 2.036(3) . ?
Rh1 O3 2.036(2) . ?
Rh1 N1 2.237(3) . ?
Rh1 Rh1 2.3951(5) 2_657 ?
O2 C1 1.261(4) . ?
O1 C1 1.267(4) 2_657 ?
O3 C7 1.254(4) . ?
O4 C7 1.259(5) 2_657 ?
N1 C17 1.330(5) . ?
N1 C13 1.333(5) . ?
C1 O1 1.267(4) 2_657 ?
C1 C2 1.495(5) . ?
C2 C3 1.520(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.513(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.520(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.512(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 O4 1.259(4) 2_657 ?
C7 C8 1.517(5) . ?
C8 C9 1.503(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.477(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.346(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 C11 1.504(9) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.374(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.372(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.382(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(5) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
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 O2 C1 O1 0.2(5) . . . 2_657 ?
Rh1 O2 C1 C2 179.1(2) . . . . ?
O2 C1 C2 C3 5.5(5) . . . . ?
O1 C1 C2 C3 -175.5(3) 2_657 . . . ?
C1 C2 C3 C4 -180.0(3) . . . . ?
C2 C3 C4 C5 176.5(3) . . . . ?
C3 C4 C5 C6 -176.1(3) . . . . ?
Rh1 O3 C7 O4 -2.1(5) . . . 2_657 ?
Rh1 O3 C7 C8 177.7(2) . . . . ?
O3 C7 C8 C9 -50.9(5) . . . . ?
O4 C7 C8 C9 128.9(4) 2_657 . . . ?
C7 C8 C9 C10 -54.5(6) . . . . ?
C8 C9 C10 C11 -78.5(9) . . . . ?
C17 N1 C13 C14 -0.6(5) . . . . ?
Rh1 N1 C13 C14 179.4(3) . . . . ?
N1 C13 C14 C15 1.0(6) . . . . ?
C13 C14 C15 C16 -0.5(6) . . . . ?
C14 C15 C16 C17 -0.2(6) . . . . ?
C13 N1 C17 C16 -0.1(5) . . . . ?
Rh1 N1 C17 C16 179.8(3) . . . . ?
C15 C16 C17 N1 0.6(6) . . . . ?
C9 C10 C11 C12 174.4(7) . . . . ?
