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_7123221
_publ_section_title
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 A photochemical route to a square planar, ruthenium(iv)-bis(imide)
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01019J
_journal_year                    2019
_chemical_formula_moiety         'C41 H55 N P4 Ru, C5 H12'
_chemical_formula_sum            'C46 H67 N P4 Ru'
_chemical_formula_weight         858.95
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                62.1820(10)
_cell_angle_beta                 81.7800(10)
_cell_angle_gamma                69.4340(10)
_cell_formula_units_Z            2
_cell_length_a                   12.33660(10)
_cell_length_b                   15.1621(2)
_cell_length_c                   15.7443(2)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    173.02
_cell_measurement_theta_max      69.99
_cell_measurement_theta_min      3.17
_cell_volume                     2437.84(6)
_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, G.M. (2015). Acta Cryst. A71, 3-8)'
_diffrn_ambient_temperature      173.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34591
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.245
_diffrn_reflns_theta_min         3.175
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.050
_exptl_absorpt_correction_T_max  0.4684
_exptl_absorpt_correction_T_min  0.3338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1502 before and 0.0847 after correction. The Ratio of minimum to maximum transmission is 0.7126. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8953
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0845P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7882
_reflns_number_total             8953
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01019j2.cif
_cod_data_source_block           final_a
_cod_database_code               7123221
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.352
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9AA-C1AA
 2.2 with sigma of 0.02
 C4AA-C6AA
 1.55 with sigma of 0.02
 C0AA-C5AA
 1.55 with sigma of 0.02
 C4AA-C8AA
 1.5 with sigma of 0.02
 C8AA-C0AA
 1.5 with sigma of 0.02
 C5AA-C0AA
 1.6 with sigma of 0.02
 C1AA-C9AA
 2.4 with sigma of 0.02
 C1AA-C1BA
 1.55 with sigma of 0.02
 C7AA-C2AA
 1.55 with sigma of 0.02
 C9AA-C2AA
 1.55 with sigma of 0.02
 C1BA-C9AA
 1.55 with sigma of 0.02
3. Others
 Fixed Sof: C5AA(0.5) H5AA(0.5) H5AB(0.5) H5AC(0.5) C9AA(0.5) H9AA(0.5)
 H9AB(0.5) C1BA(0.5) H1BA(0.5) H1BB(0.5) C6AA(0.5) H6AA(0.5) H6AB(0.5)
 H6AC(0.5) C7AA(0.5) H7AA(0.5) H7AB(0.5) H7AC(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) C8AA(0.5) H8AA(0.5) H8AB(0.5) C2AA(0.5) H2AA(0.5) H2AB(0.5)
 C4AA(0.5) H4AA(0.5) H4AB(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5)
4.a Fixed occupancy and ADP/Uiso:
 C9AA, C1BA, C0AA, C8AA, C2AA, C4AA
4.b Riding coordinates:
 C5AA(H5AA,H5AB,H5AC), C9AA(H9AA,H9AB), C1BA(H1BA,H1BB), C6AA(H6AA,H6AB,H6AC),
 C7AA(H7AA,H7AB,H7AC), C0AA(H0AA,H0AB), C8AA(H8AA,H8AB), C2AA(H2AA,H2AB),
 C4AA(H4AA,H4AB), C1AA(H1AA,H1AB,H1AC)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
4.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C21(H21), C22(H22), C15(H15), C13(H13), C5(H5), C17(H17), C14(H14),
 C40(H40), C32(H32), C23(H23), C24(H24), C25(H25), C37(H37), C41(H41), C39(H39),
  C38(H38), C33(H33), C16(H16), C29(H29), C31(H31), C30(H30)
4.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C35(H35A,H35B,H35C), C27(H27A,H27B,
 H27C), C18(H18A,H18B,H18C), C34(H34A,H34B,H34C), C26(H26A,H26B,H26C), C19(H19A,
 H19B,H19C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C)
;
_olex2_submission_special_instructions 'No special instructions were received'