A photochemical route to a square planar, ruthenium(iv)-bis(imide)
Aldrich, Kelly E.; Odom, Aaron L.; Chemical Communications  (2019) –; doi:10.1039/C9CC01019J

data_7123225
_publ_section_title
;
 A photochemical route to a square planar, ruthenium(iv)-bis(imide)
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01019J
_journal_year                    2019
_chemical_formula_moiety         'C33 H61 N4 P3 Ru'
_chemical_formula_sum            'C33 H61 N4 P3 Ru'
_chemical_formula_weight         707.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-01 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.103(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1827(16)
_cell_length_b                   18.134(2)
_cell_length_c                   17.774(2)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.24
_cell_volume                     3732.3(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      173.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31867
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.045
_diffrn_reflns_theta_min         1.647
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.4467
_exptl_absorpt_correction_T_min  0.3804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0659 before and 0.0581 after correction. The Ratio of minimum to maximum transmission is 0.8516. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.214
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0325P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4848
_reflns_number_total             7305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01019j2.cif
_cod_data_source_block           p21_c_a
_cod_original_cell_volume        3732.2(8)
_cod_database_code               7123225
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.814
_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.a Ternary CH refined with riding coordinates:
 C10(H10), C7(H7), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C5(H5), C4(H4), C17(H17), C16(H16)
2.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C8(H8A,
 H8B,H8C), C30(H30A,H30B,H30C), C24(H24A,H24B,H24C), C33(H33A,H33B,H33C),
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C32(H32A,H32B,H32C), C21(H21A,H21B,H21C),
  C28(H28A,H28B,H28C), C25(H25A,H25B,H25C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'