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_7123227
_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         'C36 H67 N4 P3 Ru, 1.25(C6 H18 O Si2)'
_chemical_formula_sum            'C43.5 H89.5 N4 O1.25 P3 Ru Si2.5'
_chemical_formula_weight         952.89
_chemical_name_systematic
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 ?
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_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
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
;
2019-02-01 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
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_cell_angle_alpha                89.860(2)
_cell_angle_beta                 69.187(2)
_cell_angle_gamma                89.450(2)
_cell_formula_units_Z            4
_cell_length_a                   17.0772(12)
_cell_length_b                   17.6205(13)
_cell_length_c                   19.6308(14)
_cell_measurement_reflns_used    9731
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      2.41
_cell_volume                     5521.4(7)
_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      173.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.965
_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  0.1483
_diffrn_reflns_av_unetI/netI     0.1096
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            74258
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.254
_diffrn_reflns_theta_min         2.408
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.884
_exptl_absorpt_correction_T_max  0.3924
_exptl_absorpt_correction_T_min  0.2333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1180 before and 0.0779 after correction. The Ratio of minimum to maximum transmission is 0.5945. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       plate
_exptl_crystal_F_000             2050
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         19537
_refine_ls_number_restraints     526
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0647P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11478
_reflns_number_total             19537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01019j2.cif
_cod_data_source_block           early_a
_cod_original_formula_sum        'C43.50 H89.50 N4 O1.25 P3 Ru Si2.50'
_cod_database_code               7123227
_shelxl_version_number           2013-3
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C10-C11B
 1.55 with sigma of 0.02
 C10-C4 \\sim C10-C12B \\sim C10-C11A \\sim C10-C11B \\sim C10-C12A
 with sigma of 0.02
 O3A-Si4 \\sim O3A-Si5A
 with sigma of 0.02
 O3B-Si4 \\sim O3B-Si5B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Si4) = Uanis(O3A) = Uanis(Si5B)
Uanis(C87B) = Uanis(O3B)
Uanis(C11B) = Uanis(C11A) = Uanis(C12B) = Uanis(C12A)
Uanis(Si2B) = Uanis(Si2A)
Uanis(C78B) = Uanis(C78A) = Uanis(C77B) = Uanis(C77A)
Uanis(O3B) = Uanis(O3A)
Uanis(Si5B) = Uanis(Si5A)
Uanis(C85) = Uanis(C86) = Uanis(C84) = Uanis(C82) = Uanis(C83)
Uanis(C87A) = Uanis(C87B)
4. Rigid body (RIGU) restrains
 Si4, O3B, C87B, Si5B, C84, C82, C85, C86, O3A, C87A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C48, C46, C47, C45, C43, C44, C51, C49, C50, C37, C42, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12B, C10, C11A, C4, C3, C5, C6, C13, C14, C15, C2, C9, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C86, C87A, C85, Si4, O3B, C84, C82, Si5B, C87B, O3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27, C25, C24, C22, C23, C18, C19, C20, C21, C16, C17, C26, C8, C7, C9, C2,
 C1, C6, C13, C15, C14, C5, C4, C3, C12A, C12B, C10, C11B, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Si5B, Si4, O3B, C84, C82, O3A, C83, H84A, H84B, H84C, H82C, H82B, H82A, Si5A,
 H83C, H83B, H83A, C85, C86, C87B, H85C, H85F, H85D, C87A, H85A, H85B, H85E,
 H86A, H86B, H86C, H86F, H86E, H86D, H87F, H87D, H87E, H87A, H87C, H87B, O1,
 Si1, C75, C74, C73, Si2A, Si2B, H75C, H75B, H75A, H74A, H74C, H74B, H73A, H73C,
  H73B, C76, C77A, C78A, C78B, C77B, H77D, H77C, H77A, H77B, H78E, H78D, H78F,
 H78B, H78A, H78C, H77E, H77F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Si5B(0.5) O3B(0.5) H85A(0.5) H85B(0.5) H85C(0.5) H85D(0.5)
 H85E(0.5) H85F(0.5) H10(0.5) H10A(0.5) C12B(0.5) H12A(0.5) H12B(0.5) H12C(0.5)
 C11A(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C87A(0.5) H87A(0.5) H87B(0.5)
 H87C(0.5) H86A(0.5) H86B(0.5) H86C(0.5) H86D(0.5) H86E(0.5) H86F(0.5)
 Si5A(0.5) O3A(0.5) C87B(0.5) H87D(0.5) H87E(0.5) H87F(0.5) C11B(0.5) H11D(0.5)
 H11E(0.5) H11F(0.5) C12A(0.5) H12D(0.5) H12E(0.5) H12F(0.5) Si2A(0.5)
 Si2B(0.5) H76A(0.5) H76B(0.5) H76C(0.5) H76D(0.5) H76E(0.5) H76F(0.5)
 C77A(0.5) H77A(0.5) H77B(0.5) H77C(0.5) C78B(0.5) H78A(0.5) H78B(0.5)
 H78C(0.5) C77B(0.5) H77D(0.5) H77E(0.5) H77F(0.5) C78A(0.5) H78D(0.5)
 H78E(0.5) H78F(0.5)
6.a Riding coordinates:
 C85(H85D,H85E,H85F), C87A(H87A,H87B,H87C), C82(H82A,H82B,H82C), C86(H86D,H86E,
 H86F), C87B(H87D,H87E,H87F), C83(H83A,H83B,H83C), C75(H75A,H75B,H75C),
 C74(H74A,H74B,H74C), C73(H73A,H73B,H73C), C76(H76A,H76B,H76C), C76(H76D,H76E,
 H76F), C77A(H77A,H77B,H77C), C78B(H78A,H78B,H78C), C78A(H78D,H78E,H78F)
6.b Ternary CH refined with riding coordinates:
 C61(H61), C13(H13), C58(H58), C25(H25), C7(H7), C43(H43), C22(H22), C49(H49),
 C46(H46), C10(H10), C10(H10A)
6.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C56(H56), C39(H39), C20(H20), C3(H3), C55(H55), C19(H19), C18(H18),
 C5(H5), C54(H54)
6.d Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C64(H64A,H64B,H64C), C32(H32A,H32B,H32C), C31(H31A,H31B,
 H31C), C44(H44A,H44B,H44C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C33(H33A,H33B,
 H33C), C66(H66A,H66B,H66C), C60(H60A,H60B,H60C), C67(H67A,H67B,H67C), C15(H15A,
 H15B,H15C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C59(H59A,H59B,H59C),
 C68(H68A,H68B,H68C), C72(H72A,H72B,H72C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C), C28(H28A,H28B,H28C), C51(H51A,H51B,H51C), C45(H45A,H45B,H45C), C14(H14A,
 H14B,H14C), C62(H62A,H62B,H62C), C50(H50A,H50B,H50C), C69(H69A,H69B,H69C),
 C29(H29A,H29B,H29C), C23(H23A,H23B,H23C), C65(H65A,H65B,H65C), C71(H71A,H71B,
 H71C), C35(H35A,H35B,H35C), C30(H30A,H30B,H30C), C63(H63A,H63B,H63C), C27(H27A,
 H27B,H27C), C47(H47A,H47B,H47C), C81(H81A,H81B,H81C), C48(H48A,H48B,H48C),
 C80(H80A,H80B,H80C), C79(H79A,H79B,H79C), C85(H85A,H85B,H85C), C12B(H12A,H12B,
 H12C), C11A(H11A,H11B,H11C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C),
 C11B(H11D,H11E,H11F), C12A(H12D,H12E,H12F), C77B(H77D,H77E,H77F)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'