#------------------------------------------------------------------------------
#$Date: 2019-03-28 00:10:11 +0100 (Thu 28 de Mar de 2019) $
#$Revision: 214382 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/32/7123222.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7123222
loop_
_publ_author_name
'Aldrich, Kelly E.'
'Odom, Aaron L.'
_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         'C32 H44 Cl2 P4 Ru'
_chemical_formula_sum            'C32 H44 Cl2 P4 Ru'
_chemical_formula_weight         724.52
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 106.429(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4079(19)
_cell_length_b                   8.4614(3)
_cell_length_c                   18.3999(10)
_cell_measurement_reflns_used    4412
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.31
_cell_volume                     3346.2(4)
_computing_cell_refinement       'APEX2 (BRUKER, V2012.10-0, 2012)'
_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(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13278
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.371
_diffrn_reflns_theta_min         1.895
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0703 before and 0.0614 after correction. The Ratio of minimum to maximum transmission is 0.9019. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.865
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0436
_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/[σ²(Fo²)+(0.0438P)²+8.7695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2426
_reflns_number_total             3067
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc01019j2.cif
_cod_data_source_block           c2_c_a
_cod_database_code               7123222
_shelxl_version_number           2013-3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.793
_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 Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ru1 Ru 0.5000 0.38429(5) 0.7500 0.02178(15) Uani 1 2 d S T P
Cl1 Cl 0.55492(5) 0.59768(12) 0.83446(7) 0.0422(3) Uani 1 1 d . . .
P1 P 0.58713(5) 0.42882(12) 0.69828(6) 0.0261(3) Uani 1 1 d . . .
P2 P 0.54437(5) 0.20324(12) 0.84292(6) 0.0237(2) Uani 1 1 d . . .
C1 C 0.66360(19) 0.4728(5) 0.7638(2) 0.0357(10) Uani 1 1 d . . .
H1A H 0.6588 0.5484 0.8021 0.054 Uiso 1 1 calc GR . .
H1B H 0.6906 0.5184 0.7356 0.054 Uiso 1 1 calc GR . .
H1C H 0.6823 0.3752 0.7887 0.054 Uiso 1 1 calc GR . .
C2 C 0.5766(2) 0.6100(5) 0.6422(3) 0.0364(11) Uani 1 1 d . . .
H2A H 0.5384 0.6022 0.6002 0.055 Uiso 1 1 calc GR . .
H2B H 0.6123 0.6248 0.6220 0.055 Uiso 1 1 calc GR . .
H2C H 0.5736 0.7002 0.6744 0.055 Uiso 1 1 calc GR . .
C3 C 0.61387(17) 0.2904(4) 0.6367(2) 0.0250(9) Uani 1 1 d . . .
C4 C 0.60114(18) 0.3124(5) 0.5591(2) 0.0292(9) Uani 1 1 d . . .
H4 H 0.5760 0.3989 0.5357 0.035 Uiso 1 1 calc R . .
C5 C 0.6246(2) 0.2100(5) 0.5151(2) 0.0378(11) Uani 1 1 d . . .
H5 H 0.6152 0.2265 0.4620 0.045 Uiso 1 1 calc R . .
C6 C 0.6615(2) 0.0849(6) 0.5479(3) 0.0426(12) Uani 1 1 d . . .
H6 H 0.6784 0.0166 0.5178 0.051 Uiso 1 1 calc R . .
C7 C 0.6740(2) 0.0587(5) 0.6245(3) 0.0386(11) Uani 1 1 d . . .
H7 H 0.6983 -0.0298 0.6471 0.046 Uiso 1 1 calc R . .
C8 C 0.65098(18) 0.1614(5) 0.6687(2) 0.0294(9) Uani 1 1 d . . .
H8 H 0.6606 0.1438 0.7217 0.035 Uiso 1 1 calc R . .
C9 C 0.50116(19) 0.0235(5) 0.8493(3) 0.0363(10) Uani 1 1 d . . .
H9A H 0.4584 0.0511 0.8480 0.055 Uiso 1 1 calc GR . .
H9B H 0.5212 -0.0312 0.8969 0.055 Uiso 1 1 calc GR . .
H9C H 0.5006 -0.0458 0.8065 0.055 Uiso 1 1 calc GR . .
C10 C 0.5550(2) 0.2800(6) 0.9386(2) 0.0406(11) Uani 1 1 d . . .
H10A H 0.5814 0.3744 0.9460 0.061 Uiso 1 1 calc GR . .
H10B H 0.5749 0.1993 0.9757 0.061 Uiso 1 1 calc GR . .
H10C H 0.5144 0.3077 0.9453 0.061 Uiso 1 1 calc GR . .
C11 C 0.62307(17) 0.1218(4) 0.8559(2) 0.0218(8) Uani 1 1 d . . .
C12 C 0.67475(19) 0.2101(5) 0.8946(2) 0.0316(10) Uani 1 1 d . . .
H12 H 0.6692 0.3132 0.9120 0.038 Uiso 1 1 calc R . .
C13 C 0.7340(2) 0.1488(6) 0.9079(3) 0.0404(11) Uani 1 1 d . . .
H13 H 0.7689 0.2108 0.9337 0.048 Uiso 1 1 calc R . .
C14 C 0.7428(2) -0.0008(6) 0.8840(3) 0.0426(12) Uani 1 1 d . . .
H14 H 0.7837 -0.0426 0.8934 0.051 Uiso 1 1 calc R . .
C15 C 0.6923(2) -0.0896(5) 0.8466(3) 0.0417(12) Uani 1 1 d . . .
H15 H 0.6981 -0.1935 0.8302 0.050 Uiso 1 1 calc R . .
C16 C 0.63254(19) -0.0279(5) 0.8324(2) 0.0313(10) Uani 1 1 d . . .
H16 H 0.5978 -0.0901 0.8062 0.038 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl1 Ru1 Cl1 86.13(6) 2_656 .
P1 Ru1 Cl1 79.68(4) . .
P1 Ru1 Cl1 79.68(4) 2_656 2_656
P1 Ru1 Cl1 87.29(4) 2_656 .
P1 Ru1 Cl1 87.29(4) . 2_656
P1 Ru1 P1 162.17(5) 2_656 .
P2 Ru1 Cl1 89.17(4) . .
P2 Ru1 Cl1 89.17(4) 2_656 2_656
P2 Ru1 Cl1 170.78(4) . 2_656
P2 Ru1 Cl1 170.78(4) 2_656 .
P2 Ru1 P1 99.67(4) 2_656 2_656
P2 Ru1 P1 99.67(4) . .
P2 Ru1 P1 92.20(4) . 2_656
P2 Ru1 P1 92.20(4) 2_656 .
P2 Ru1 P2 96.54(5) 2_656 .
C1 P1 Ru1 118.62(14) . .
C1 P1 C3 97.31(19) . .
C2 P1 Ru1 111.21(14) . .
C2 P1 C1 98.5(2) . .
C2 P1 C3 101.46(19) . .
C3 P1 Ru1 125.36(12) . .
C9 P2 Ru1 118.49(14) . .
C9 P2 C10 99.3(2) . .
C9 P2 C11 100.70(18) . .
C10 P2 Ru1 112.96(15) . .
C10 P2 C11 98.53(18) . .
C11 P2 Ru1 122.77(12) . .
P1 C1 H1A 109.5 . .
P1 C1 H1B 109.5 . .
P1 C1 H1C 109.5 . .
H1A C1 H1B 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
P1 C2 H2A 109.5 . .
P1 C2 H2B 109.5 . .
P1 C2 H2C 109.5 . .
H2A C2 H2B 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C4 C3 P1 122.7(3) . .
C4 C3 C8 117.6(4) . .
C8 C3 P1 119.7(3) . .
C3 C4 H4 119.5 . .
C5 C4 C3 121.0(4) . .
C5 C4 H4 119.5 . .
C4 C5 H5 119.8 . .
C6 C5 C4 120.4(4) . .
C6 C5 H5 119.8 . .
C5 C6 H6 120.1 . .
C5 C6 C7 119.8(4) . .
C7 C6 H6 120.1 . .
C6 C7 H7 120.0 . .
C6 C7 C8 120.0(4) . .
C8 C7 H7 120.0 . .
C3 C8 H8 119.4 . .
C7 C8 C3 121.2(4) . .
C7 C8 H8 119.4 . .
P2 C9 H9A 109.5 . .
P2 C9 H9B 109.5 . .
P2 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
P2 C10 H10A 109.5 . .
P2 C10 H10B 109.5 . .
P2 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 C11 P2 119.5(3) . .
C16 C11 P2 122.0(3) . .
C16 C11 C12 118.4(4) . .
C11 C12 H12 119.7 . .
C13 C12 C11 120.5(4) . .
C13 C12 H12 119.7 . .
C12 C13 H13 119.7 . .
C14 C13 C12 120.5(4) . .
C14 C13 H13 119.7 . .
C13 C14 H14 120.2 . .
C15 C14 C13 119.6(4) . .
C15 C14 H14 120.2 . .
C14 C15 H15 119.9 . .
C14 C15 C16 120.2(4) . .
C16 C15 H15 119.9 . .
C11 C16 C15 120.9(4) . .
C11 C16 H16 119.6 . .
C15 C16 H16 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 Cl1 2.4714(10) 2_656
Ru1 Cl1 2.4714(11) .
Ru1 P1 2.4311(10) 2_656
Ru1 P1 2.4311(10) .
Ru1 P2 2.3015(10) .
Ru1 P2 2.3015(10) 2_656
P1 C1 1.833(4) .
P1 C2 1.825(4) .
P1 C3 1.844(4) .
P2 C9 1.824(4) .
P2 C10 1.828(4) .
P2 C11 1.845(4) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.388(5) .
C3 C8 1.397(5) .
C4 H4 0.9500 .
C4 C5 1.387(6) .
C5 H5 0.9500 .
C5 C6 1.373(6) .
C6 H6 0.9500 .
C6 C7 1.375(6) .
C7 H7 0.9500 .
C7 C8 1.385(6) .
C8 H8 0.9500 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 C12 1.392(5) .
C11 C16 1.374(5) .
C12 H12 0.9500 .
C12 C13 1.382(6) .
C13 H13 0.9500 .
C13 C14 1.372(7) .
C14 H14 0.9500 .
C14 C15 1.371(7) .
C15 H15 0.9500 .
C15 C16 1.392(6) .
C16 H16 0.9500 .
