A robust bis-rhodium(i) complex of π-extended planar, anti-aromatic hexaphyrin[1.0.1.0.1.0].
Samala, Srinivas; Dutta, Ranjan; He, Qing; Park, Yeonju; Chandra, Brijesh; Lynch, Vincent M.; Jung, Young Mee; Sessler, Jonathan L.; Lee, Chang-Hee; Chemical communications (Cambridge, England) 56 (2020) 758–761; doi:10.1039/c9cc09221h

data_7125812
_publ_section_title
;
 A robust bis-rhodium(i) complex of \p-extended planar, anti-aromatic
 hexaphyrin[1.0.1.0.1.0].
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              758
_journal_page_last               761
_journal_paper_doi               10.1039/c9cc09221h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C67 H18.68 F15 N6 O4 Rh2'
_chemical_formula_sum            'C67 H18 F15 N6 O4 Rh2'
_chemical_formula_weight         1461.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-17 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.870(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5064(2)
_cell_length_b                   13.7489(2)
_cell_length_c                   36.4349(8)
_cell_measurement_reflns_used    10707
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      75.4620
_cell_measurement_theta_min      3.1910
_cell_volume                     5213.50(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2940
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -111.00 -17.00   1.00   11.00    --  -41.59 -38.00  60.00   94
  2  \w    -87.00  -4.00   1.00   11.00    --  -41.59 125.00 -30.00   83
  3  \w    -65.00  26.00   1.00   11.00    --  -41.59  38.00-120.00   91
  4  \w    -67.00  31.00   1.00   11.00    --  -41.59  57.00 -30.00   98
  5  \w     58.00  92.00   1.00   11.00    --   41.59-125.00-150.00   34
  6  \w     42.00  72.00   1.00   35.00    --  112.00 -15.00-120.00   30
  7  \w     43.00 140.00   1.00   35.00    --  112.00 -30.00 -30.00   97
  8  \w     45.00  86.00   1.00   35.00    --  112.00 -94.00 -30.00   41
  9  \w     42.00 140.00   1.00   35.00    --  112.00 -77.00   0.00   98
 10  \w     64.00 117.00   1.00   35.00    --  112.00-125.00-180.00   53
 11  \w    100.00 173.00   1.00   35.00    --  112.00 125.00 -60.00   73
 12  \w     98.00 167.00   1.00   35.00    --  112.00  30.00-150.00   69
 13  \w     39.00 118.00   1.00   35.00    --  112.00-125.00  30.00   79
 14  \w     97.00 151.00   1.00   35.00    --  112.00 125.00  60.00   54
 15  \w     80.00 117.00   1.00   35.00    --  112.00-125.00 -90.00   37
 16  \w     94.00 178.00   1.00   35.00    --  112.00 125.00  30.00   84
 17  \w     45.00 110.00   1.00   35.00    --  112.00 -45.00 150.00   65
 18  \w     87.00 178.00   1.00   35.00    --  112.00  45.00 150.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0283426000
_diffrn_orient_matrix_UB_12      0.0516443000
_diffrn_orient_matrix_UB_13      -0.0004353000
_diffrn_orient_matrix_UB_21      0.0619897000
_diffrn_orient_matrix_UB_22      -0.0210768000
_diffrn_orient_matrix_UB_23      -0.0114846000
_diffrn_orient_matrix_UB_31      -0.0292299000
_diffrn_orient_matrix_UB_32      0.0054079000
_diffrn_orient_matrix_UB_33      -0.0411039000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            37729
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.587
_diffrn_reflns_theta_min         3.440
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_description       block
_exptl_crystal_F_000             2876
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.054
_refine_diff_density_max         2.295
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         10637
_refine_ls_number_restraints     1142
_refine_ls_restrained_S_all      2.889
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0929
_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/[\s^2^(Fo^2^)+(0.0754P)^2^+38.8196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2224
_refine_ls_wR_factor_ref         0.2295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9259
_reflns_number_total             10637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09221h2.cif
_cod_data_source_block           BiRhcomplex3
_cod_depositor_comments          'Adding full bibliography for 7125812.cif.'
_cod_database_code               7125812
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C80H60N8O8Rh2
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Others
 Fixed Sof: H1(0.68) Rh1(0.68) Rh2(0.68) O1A(0.68) C1A(0.68) C2A(0.68)
 O2A(0.68) O3A(0.68) C3A(0.68) O4A(0.68) C4A(0.68) Rh3(0.32) Rh4(0.32)
 O5A(0.32) C5A(0.32) O6A(0.32) C6A(0.32) O7A(0.32) C7A(0.32) O8A(0.32)
 C8A(0.32) F6(0.58) F7(0.58) F8(0.58) F9(0.58) F10(0.58) C46(0.58) C47(0.58)
 C48(0.58) C49(0.58) C50(0.58) C51(0.58) F6A(0.42) F7A(0.42) F8A(0.42)
 F9A(0.42) F10A(0.42) C46A(0.42) C47A(0.42) C48A(0.42) C49A(0.42) C50A(0.42)
 C51A(0.42)
 Fixed Uiso: H2(0.046) H7(0.051) H11(0.049) H16(0.052) H20(0.055) H25(0.05)
 H29(0.047) H30(0.049) H31(0.052) H32(0.052) H41(0.052) H42(0.065) H43(0.06)
 H44(0.049) H53(0.05) H54(0.054) H55(0.047) H56(0.044) H1(0.061)
 Fixed X: H2(0.617209) H7(0.837006) H11(0.554847) H16(0.032502) H20(-0.152844)
 H25(0.144671) H29(0.8328) H30(1.029909) H31(1.109594) H32(0.985753)
 H41(0.46347) H42(0.35673) H43(0.174557) H44(0.09521) H53(-0.279634) H54(-
 0.374404) H55(-0.266996) H56(-0.068329) H1(0.416781)
 Fixed Y: H2(0.254423) H7(0.597353) H11(0.919196) H16(1.019397) H20(0.743892)
 H25(0.294788) H29(0.22672) H30(0.205734) H31(0.322865) H32(0.459749)
 H41(1.088924) H42(1.235283) H43(1.264834) H44(1.144768) H53(0.607672)
 H54(0.47968) H55(0.331433) H56(0.30946) H1(0.496261)
 Fixed Z: H2(0.413812) H7(0.297721) H11(0.259994) H16(0.351466) H20(0.433931)
 H25(0.454573) H29(0.395723) H30(0.375848) H31(0.338062) H32(0.319084)
 H41(0.25457) H42(0.245219) H43(0.274589) H44(0.308729) H53(0.457379)
 H54(0.485883) H55(0.495495) H56(0.476287) H1(0.384399)
;
_shelx_res_checksum              88849
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.941
_oxdiff_exptl_absorpt_empirical_full_min 0.717