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_7123223
_publ_section_title
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 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         'C30 H52 N2 P2 Ru'
_chemical_formula_sum            'C30 H52 N2 P2 Ru'
_chemical_formula_weight         603.74
_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   geom
_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                65.8160(10)
_cell_angle_beta                 77.352(2)
_cell_angle_gamma                68.2570(10)
_cell_formula_units_Z            1
_cell_length_a                   9.2674(2)
_cell_length_b                   9.4247(2)
_cell_length_c                   11.0702(2)
_cell_measurement_reflns_used    4565
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.02
_cell_measurement_theta_min      4.39
_cell_volume                     816.70(3)
_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
'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_diffrn_ambient_temperature      173.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12542
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.069
_diffrn_reflns_theta_min         4.392
_exptl_absorpt_coefficient_mu    4.939
_exptl_absorpt_correction_T_max  0.5235
_exptl_absorpt_correction_T_min  0.3505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0900 before and 0.0690 after correction. The Ratio of minimum to maximum transmission is 0.6695. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.397
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0460P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2743
_reflns_number_total             3103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01019j2.cif
_cod_data_source_block           p1-_a
_cod_original_cell_volume        816.71(3)
_cod_database_code               7123223
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.480
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C), C11(H11A,H11B,
 H11C), C14(H14A,H14B,H14C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'