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_7129263
_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_absolute_configuration rmad
_chemical_formula_moiety         'C44 H27 N4 O2 Rh'
_chemical_formula_sum            'C44 H27 N4 O2 Rh'
_chemical_formula_weight         746.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-13 deposited with the CCDC.	2021-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1380(15)
_cell_length_b                   6.6176(4)
_cell_length_c                   22.4596(11)
_cell_measurement_reflns_used    5209
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      51.92
_cell_measurement_theta_min      3.47
_cell_volume                     3290.3(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      193.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1693
_diffrn_reflns_av_unetI/netI     0.1413
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31791
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.295
_diffrn_reflns_theta_min         3.474
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.037
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1846 before and 0.1004 after correction. The Ratio of minimum to maximum transmission is 0.7290. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.877
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.24(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         5774
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1693
_refine_ls_R_factor_gt           0.0977
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1673P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2850
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                3292
_reflns_number_total             5774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05641g2.cif
_cod_data_source_block           2108111829
_cod_database_code               7129263
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.76(4)
 0.24(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained distances
 Rh1-C2 \\sim Rh2-C3 \\sim Rh2-C4 \\sim Rh1-C1
 with sigma of 0.02
4. Rigid bond restraints
 C37, C38
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim C1 \\sim C2 \\sim C4: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
O2 \\sim C2 \\sim C3: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Sof(H1)=Sof(Rh2)=Sof(C3)=Sof(C4)=1-FVAR(1)
 Sof(H3)=Sof(Rh1)=Sof(C1)=Sof(C2)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), C6(H6), C7(H7), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C18(H18), C21(H21), C22(H22), C26(H26), C27(H27), C30(H30), C31(H31),
  C32(H32), C33(H33), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
 C46(H46), C45(H45), C44(H44), C43(H43), C42(H42)
7.b Fitted hexagon refined as free rotating group:
 C35(C36,C37,C38,C39,C40), C41(C46,C45,C44,C43,C42)
;
_shelx_res_checksum              29218
_olex2_submission_special_instructions 'No special instructions were received'