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_7123224
_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         '12(C15 H26 N P)'
_chemical_formula_sum            'C180 H312 N12 P12'
_chemical_formula_weight         3016.04
_chemical_name_systematic
;
 ?
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_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_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
;
2019-02-02 deposited with the CCDC.    2019-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   13.4178(8)
_cell_length_b                   20.5314(11)
_cell_length_c                   17.4463(12)
_cell_measurement_reflns_used    4393
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.036
_cell_measurement_theta_min      3.934
_cell_volume                     4806.2(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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, 2008)'
_diffrn_ambient_temperature      173.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1413
_diffrn_reflns_av_unetI/netI     0.1385
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26930
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.196
_diffrn_reflns_theta_min         3.294
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0800 before and 0.0608 after correction. The Ratio of minimum to maximum transmission is 0.8873. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 1113 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         8822
_refine_ls_number_restraints     412
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.2024
_refine_ls_R_factor_gt           0.0951
_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^)+(0.0959P)^2^+2.2610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2092
_refine_ls_wR_factor_ref         0.2672
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4032
_reflns_number_total             8822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01019j2.cif
_cod_data_source_block           pna21
_cod_database_code               7123224
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.828
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(10)
 0.51(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C40B-C36B
 1.53 with sigma of 0.02
 C32B-C37B
 1.46 with sigma of 0.02
 C38B-C37B = C37B-C39B
 1.55 with sigma of 0.02
 C39B-C37B
 1.55 with sigma of 0.02
 C42B-C41B
 2.57 with sigma of 0.04
 C32B-C39B
 2.55 with sigma of 0.04
 C39B-C38B
 2.55 with sigma of 0.04
 C39B-C32B
 2.7 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) =
Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21)
Uanis(C15B) = Uanis(C14A) = Uanis(C14B) = Uanis(C13A) = Uanis(C13B) =
Uanis(C15A)
Uanis(C29A) = Uanis(C29B) = Uanis(C30B) = Uanis(C30A) = Uanis(C28A) =
Uanis(C28B)
Uanis(N3B) = Uanis(N3A)
Uanis(C36B) = Uanis(C31B) = Uanis(C32B) = Uanis(C33B) = Uanis(C34B) =
Uanis(C35B)
Uanis(C34A) = Uanis(C35A) = Uanis(C36A) = Uanis(C31A) = Uanis(C32A) =
Uanis(C33A)
5. Rigid body (RIGU) restrains
 C8, C9, C7, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C10, C12, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41B, C42B, C40B, C36B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38B, C37B, C39B, C32B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C7, C9, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27, C25, C26, C21, C16, C17, C18, C19, C20, C22, C24, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C7, C9, C2, C3, C4, C5, C6, C1, C10, C12, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C38B, C37B, C39B, C32B, C31B, C36B, C35B, C34B, C33B, C40B, C41B, C42B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31A, P3, C45, N3A, C43, C44, N3B, C31B, C36A, C32A, C32B, C36B, C40A, C35A,
 C37A, C33A, C37B, C33B, C40B, C35B, C42A, C41A, C34A, C42B, C38A, C39A, C38B,
 C39B, C34B, C41B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N3A(0.5) C28B(0.45) H28A(0.45) H28B(0.45) H28C(0.45) C37B(0.5)
 H37B(0.5) C14A(0.55) H14A(0.55) H14B(0.55) H14C(0.55) C40B(0.5) H40B(0.5)
 C15A(0.55) H15A(0.55) H15B(0.55) H15C(0.55) C30A(0.45) H30A(0.45) H30B(0.45)
 H30C(0.45) C32B(0.5) C33B(0.5) H33B(0.5) C34B(0.5) H34B(0.5) C35B(0.5)
 H35B(0.5) C36B(0.5) C31B(0.5) C13A(0.55) H13A(0.55) H13B(0.55) H13C(0.55)
 C29A(0.45) H29A(0.45) H29B(0.45) H29C(0.45) C42B(0.5) H42A(0.5) H42B(0.5)
 H42C(0.5) C41B(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C38B(0.5) H38A(0.5)
 H38B(0.5) H38C(0.5) C15B(0.45) H15D(0.45) H15E(0.45) H15F(0.45) C14B(0.45)
 H14D(0.45) H14E(0.45) H14F(0.45) C13B(0.45) H13D(0.45) H13E(0.45) H13F(0.45)
 C39B(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C28A(0.55) H28D(0.55) H28E(0.55)
 H28F(0.55) C30B(0.55) H30D(0.55) H30E(0.55) H30F(0.55) C29B(0.55) H29D(0.55)
 H29E(0.55) H29F(0.55) N3B(0.5) C40A(0.5) H40A(0.5) C42A(0.5) H42D(0.5)
 H42E(0.5) H42F(0.5) C37A(0.5) H37A(0.5) C38A(0.5) H38D(0.5) H38E(0.5)
 H38F(0.5) C41A(0.5) H41D(0.5) H41E(0.5) H41F(0.5) C34A(0.5) H34A(0.5)
 C35A(0.5) H35A(0.5) C36A(0.5) C31A(0.5) C32A(0.5) C33A(0.5) H33A(0.5)
 C39A(0.5) H39D(0.5) H39E(0.5) H39F(0.5)
7.a Riding coordinates:
 C20(H20), C19(H19), C18(H18), C4(H4), C5(H5), C3(H3), C45(H45A,H45B,H45C),
 C10(H10), C28B(H28A,H28B,H28C), C37B(H37B), C14A(H14A,H14B,H14C), C7(H7),
 C40B(H40B), C15A(H15A,H15B,H15C), C30A(H30A,H30B,H30C), C43(H43A,H43B,H43C),
 C25(H25), C22(H22), C33B(H33B), C34B(H34B), C35B(H35B), C44(H44A,H44B,H44C),
 C13A(H13A,H13B,H13C), C29A(H29A,H29B,H29C), C12(H12A,H12B,H12C), C23(H23A,H23B,
 H23C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C24(H24A,H24B,
 H24C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C42B(H42A,H42B,H42C),
 C41B(H41A,H41B,H41C), C38B(H38A,H38B,H38C), C15B(H15D,H15E,H15F), C14B(H14D,
 H14E,H14F), C13B(H13D,H13E,H13F), C39B(H39A,H39B,H39C), C28A(H28D,H28E,H28F),
 C30B(H30D,H30E,H30F), C29B(H29D,H29E,H29F), C40A(H40A), C42A(H42D,H42E,H42F),
 C37A(H37A), C38A(H38D,H38E,H38F), C41A(H41D,H41E,H41F), C34A(H34A), C35A(H35A),
  C33A(H33A), C39A(H39D,H39E,H39F)
7.b Fitted hexagon refined as free rotating group:
 C4(C5,C6,C1,C2,C3), C32B(C33B,C34B,C35B,C36B,C31B), C34A(C35A,C36A,C31A,C32A,
 C33A)
;
_olex2_submission_special_instructions 'No special instructions were received'