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_7710521
_publ_section_title
;
 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         'C77 H52 N4 O P Ru'
_chemical_formula_sum            'C77 H52 N4 O P Ru'
_chemical_formula_weight         1181.26
_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
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 97.4850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.57760(10)
_cell_length_b                   26.8909(3)
_cell_length_c                   22.0304(2)
_cell_measurement_reflns_used    1151121
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.840
_cell_measurement_theta_min      1.76
_cell_volume                     5625.59(10)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  MX2/LNLS
_diffrn_measurement_method       \phi
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82665
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            115112
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        29.710
_diffrn_reflns_theta_max         29.840
_diffrn_reflns_theta_min         1.760
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.857
_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    1.395
_exptl_crystal_description       needle
_exptl_crystal_F_000             2436
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.167
_refine_diff_density_min         -2.171
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         9777
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0994
_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^)+(0.0045P)^2^+72.0330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8882
_reflns_number_total             9777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01095j2.cif
_cod_data_source_block           shelxt
_cod_database_code               7710521
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.900
_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
 O1-C77
 1.41 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C77) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C51(H51), C8(H8), C18(H18), C52(H52), C49(H49), C68(H68), C54(H54),
 C48(H48), C2(H2), C10(H10), C76(H76), C60(H60), C17(H17), C12(H12), C29(H29),
 C66(H66), C7(H7), C3(H3), C46(H46), C67(H67), C13(H13), C31(H31), C22(H22),
 C70(H70), C72(H72), C32(H32), C75(H75), C23(H23), C38(H38), C57(H57), C28(H28),
  C62(H62), C55(H55), C61(H61), C43(H43), C24(H24), C25(H25), C56(H56),
 C74(H74), C69(H69), C63(H63), C73(H73), C64(H64), C44(H44), C35(H35), C40(H40),
  C39(H39), C34(H34)
4.b Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C)
;
_shelx_res_checksum              61913
_olex2_submission_special_instructions 'No special instructions were received'