A synthetic tactic to substitute axial ligands in sterically demanding Ru(ii)porphyrinates
Fontana, Liniquer A.; Rigolin, Vitor H.; Ribeiro, Marcos A.; Barros, Wdeson P.; Megiatto, Jackson D.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01095J

data_7710522
_publ_section_title
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 A synthetic tactic to substitute axial ligands in sterically demanding
 Ru(ii)porphyrinates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01095J
_journal_year                    2022
_chemical_formula_moiety
'C62 H46 N4 O2 Ru S2, C H3 O0.486 S0.486, C H3 O0.514 S0.514'
_chemical_formula_sum            'C64 H52 N4 O3 Ru S3'
_chemical_formula_weight         1122.34
_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
_audit_creation_date             2022-05-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-18 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                104.4200(10)
_cell_angle_beta                 90.0060(10)
_cell_angle_gamma                100.4600(10)
_cell_formula_units_Z            2
_cell_length_a                   9.05560(10)
_cell_length_b                   14.09280(10)
_cell_length_c                   20.61510(10)
_cell_measurement_reflns_used    14976
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.4221106457
_cell_measurement_theta_min      1.78126439649
_cell_volume                     2502.81(4)
_computing_data_collection       MXCube
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    XT
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'MX2 LNLS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82602
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.889
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52098
_diffrn_reflns_point_group_measured_fraction_full 0.889
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        29.710
_diffrn_reflns_theta_max         29.839
_diffrn_reflns_theta_min         2.374
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.938
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         8075
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+2.6776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7370
_reflns_number_total             8075
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01095j2.cif
_cod_data_source_block           shelxt_CCDC1
_cod_database_code               7710522
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S4-C66 = S3-C65 = S4-C63 = S3-C64
 1.8 with sigma of 0.02
 C66-C63
 2.7 with sigma of 0.04
 C64-C65
 2.7 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C66) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C65)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(S4)=Sof(O3)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C65)=Sof(H65A)=
 Sof(H65B)=Sof(H65C)=1-FVAR(1)
 Sof(S3)=Sof(O4)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C63)=Sof(H63A)=
 Sof(H63B)=Sof(H63C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C20(H20), C57(H57), C17(H17), C32(H32), C7(H7), C2(H2),
 C3(H3), C13(H13), C46(H46), C18(H18), C56(H56), C22(H22), C31(H31), C54(H54),
 C38(H38), C40(H40), C12(H12), C43(H43), C34(H34), C35(H35), C39(H39), C51(H51),
  C55(H55), C52(H52), C49(H49), C25(H25), C48(H48), C44(H44), C24(H24),
 C29(H29), C28(H28), C23(H23)
5.b Idealised Me refined as rotating group:
 C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,
 H62C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C65(H65A,H65B,H65C), C63(H63A,
 H63B,H63C)
;
_shelx_res_checksum              41366
_olex2_submission_special_instructions 'No special instructions were received'