Porphyrin(2.1.2.1) as a novel binucleating ligand: synthesis and molecular structures of mono- and di-rhodium(i) complexes
Xue, Songlin; Liu, Ningchao; Mei, Peifeng; Kuzuhara, Daiki; Zhou, Mingbo; Pan, Jianming; Yamada, Hiroko; Qiu, Fengxian; Chemical Communications  (2021) –; doi:10.1039/D1CC05641G

data_7129262
_publ_section_title
;
 Porphyrin(2.1.2.1) as a novel binucleating ligand: synthesis and
 molecular structures of mono- and di-rhodium(i) complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05641G
_journal_year                    2021
_chemical_formula_moiety         'C46 H26 N4 O4 Rh2'
_chemical_formula_sum            'C46 H26 N4 O4 Rh2'
_chemical_formula_weight         904.53
_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     dual
_audit_creation_date             2021-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-19 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.341(2)
_cell_angle_beta                 104.620(2)
_cell_angle_gamma                98.347(2)
_cell_formula_units_Z            6
_cell_length_a                   13.6924(12)
_cell_length_b                   18.0240(17)
_cell_length_c                   26.204(2)
_cell_measurement_reflns_used    8874
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.716
_cell_measurement_theta_min      2.325
_cell_volume                     6185.1(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            53450
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.130
_diffrn_reflns_theta_min         1.555
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0963 before and 0.0394 after correction. The Ratio of minimum to maximum transmission is 0.8521. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1513
_refine_ls_number_reflns         30021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0495
_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/[\s^2^(Fo^2^)+(0.0568P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16332
_reflns_number_total             30021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05641g2.cif
_cod_data_source_block           mo_2106021996_0m
_cod_original_cell_volume        6185.2(10)
_cod_database_code               7129262
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
  C32(H32), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
 C42(H42), C43(H43), C44(H44), C51(H51), C52(H52), C59(H59), C60(H60), C62(H62),
  C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C73(H73),
 C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C81(H81), C82(H82), C83(H83),
  C84(H84), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C97(H97),
 C98(H98), C105(H105), C106(H106), C108(H108), C109(H109), C110(H110),
 C111(H111), C112(H112), C113(H113), C114(H114), C119(H119), C120(H120),
 C121(H121), C122(H122), C123(H123), C124(H124), C127(H127), C128(H128),
 C129(H129), C130(H130), C132(H132), C133(H133), C134(H134), C135(H135),
 C136(H136)
;
_shelx_res_checksum              30756
_shelx_fab_checksum              26087
_olex2_submission_special_instructions 'No special instructions were received'