Mix and (Mis)match: further studies of the electronic structure and mixed-valence characteristics of 1,4-diethynylbenzene-bridged bimetallic complexes.
Safari, Parvin; Moggach, Stephen A.; Low, Paul J.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9835–9848; doi:10.1039/d0dt01794a

data_7704719
_publ_section_title
;
 Mix and (Mis)match: further studies of the electronic structure and
 mixed-valence characteristics of 1,4-diethynylbenzene-bridged bimetallic
 complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9835
_journal_page_last               9848
_journal_paper_doi               10.1039/d0dt01794a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C59 H55 O3 P2 Ru W'
_chemical_formula_sum            'C59 H55 O3 P2 Ru W'
_chemical_formula_weight         1158.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-08 deposited with the CCDC.	2020-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.409(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6530(18)
_cell_length_b                   22.4069(19)
_cell_length_c                   16.827(3)
_cell_measurement_reflns_used    2787
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      49.4500
_cell_measurement_theta_min      3.6920
_cell_volume                     5178.0(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.665
_diffrn_measured_fraction_theta_max 0.666
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  62.00   0.50    5.00    --   46.07 -59.00  37.00  174
  2  \w     30.00 118.00   0.50   15.00    --  102.41 -59.00  37.00  176
  3  \w     37.00 118.00   0.50   15.00    --  102.41 -61.00 -90.00  162
  4  \w     54.00  98.00   0.50   15.00    --  102.41 -94.00-120.00   88
  5  \w     31.00 119.00   0.50   15.00    --  102.41 -61.00  30.00  176
  6  \w     31.00 118.00   0.50    5.00    --   46.07  59.00 177.00  174
  7  \w     87.00 175.00   0.50   15.00    --  102.41  59.00 177.00  176
  8  \w     88.00 174.00   0.50   15.00    --  102.41  61.00 150.00  172
  9  \w    129.00 173.00   0.50   15.00    --  102.41  77.00 -90.00   88
 10  \w     81.00 106.00   0.50   15.00    --  102.41  77.00 -90.00   50
 11  \w     34.00 119.00   0.50    5.00    --   46.07  38.00 -60.00  170
 12  \w     24.00 118.00   0.50    5.00    --   46.07  77.00 -30.00  188
 13  \w     34.00 121.00   0.50    5.00    --   46.07  19.00 150.00  174
 14  \w     31.00  99.00   0.50   15.00    --  102.41 -94.00  60.00  136
 15  \w    -62.00  26.00   0.50    5.00    --  -46.07  59.00 177.00  176
 16  \w   -105.00 -80.00   0.50   15.00    -- -102.41 -77.00 -51.51   50
 17  \w   -107.00 -81.00   0.50   15.00    -- -102.41 -73.00 -70.96   52
 18  \w   -109.00 -83.00   0.50   15.00    -- -102.41 -69.00 -38.52   52
 19  \w   -116.00 -89.00   0.50   15.00    -- -102.41 -47.00 -69.98   54
 20  \w   -119.00 -90.00   0.50   15.00    -- -102.41 -30.00 -60.00   58
 21  \w   -117.00 -30.00   0.50    5.00    --  -46.07 -59.00  37.00  174
 22  \w   -118.00 -30.00   0.50   15.00    -- -102.41  59.00 177.00  176
 23  \w   -115.00 -31.00   0.50   15.00    -- -102.41  45.00  60.00  168
 24  \w   -118.00 -23.00   0.50    5.00    --  -46.07 -77.00-120.00  190
 25  \w   -118.00 -73.00   0.50    5.00    --  -46.07-125.00 -60.00   90
 26  \w   -118.00 -73.00   0.50    5.00    --  -46.07-125.00 -30.00   90
 27  \w   -118.00 -73.00   0.50    5.00    --  -46.07-125.00-180.00   90
 28  \w   -157.00-129.00   0.50   15.00    -- -102.41 -77.00 -51.51   56
 29  \w   -165.00 -90.00   0.50   15.00    -- -102.41 -46.00 -80.04  150
 30  \w   -175.00 -87.00   0.50   15.00    -- -102.41 -59.00  37.00  176
 31  \w   -165.00 -83.00   0.50   15.00    -- -102.41 -94.00 150.00  164
 32  \w   -175.00 -86.00   0.50   15.00    -- -102.41 -62.00  -5.13  178
 33  \w   -175.00 -84.00   0.50   15.00    -- -102.41 -67.00-170.43  182
 34  \w   -175.00 -90.00   0.50   15.00    -- -102.41 -46.00 -74.32  170
 35  \w   -175.00 -88.00   0.50   15.00    -- -102.41 -55.00 116.45  174
 36  \w   -175.00 -80.00   0.50   15.00    -- -102.41 -75.00 -20.44  190
 37  \w   -175.00 -91.00   0.50   15.00    -- -102.41 -69.00 -85.38  168
 38  \w   -176.00 -94.00   0.50   15.00    -- -102.41 -30.00-120.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0908719000
_diffrn_orient_matrix_UB_12      -0.0143413000
_diffrn_orient_matrix_UB_13      -0.0046778000
_diffrn_orient_matrix_UB_21      -0.0353967000
_diffrn_orient_matrix_UB_22      0.0449686000
_diffrn_orient_matrix_UB_23      -0.0840071000
_diffrn_orient_matrix_UB_31      -0.0058241000
_diffrn_orient_matrix_UB_32      -0.0500328000
_diffrn_orient_matrix_UB_33      -0.0741661000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1865
_diffrn_reflns_av_unetI/netI     0.1304
_diffrn_reflns_Laue_measured_fraction_full 0.665
_diffrn_reflns_Laue_measured_fraction_max 0.666
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26569
_diffrn_reflns_point_group_measured_fraction_full 0.665
_diffrn_reflns_point_group_measured_fraction_max 0.666
_diffrn_reflns_theta_full        60.599
_diffrn_reflns_theta_max         60.599
_diffrn_reflns_theta_min         3.218
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.324
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       block
_exptl_crystal_F_000             2324
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         5209
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1635
_refine_ls_R_factor_gt           0.1053
_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^)+(0.1448P)^2^+51.3354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2600
_refine_ls_wR_factor_ref         0.2978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3125
_reflns_number_total             5209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01794a2.cif
_cod_data_source_block           ps2p123
_cod_depositor_comments          'Adding full bibliography for 7704719.cif.'
_cod_original_cell_volume        5177.9(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7704719
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'W1 Ru1 C10 H58 O3 P2'
_chemical_oxdiff_usercomment     'Parvin for P Low'
_shelx_estimated_absorpt_t_max   0.763
_shelx_estimated_absorpt_t_min   0.552
_reflns_odcompleteness_completeness 60.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
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
2. Restrained distances
 C10-C5 \\sim C6-C1 \\sim C7-C2 \\sim C8-C3 \\sim C9-C4
 with sigma of 0.02
 W1-C3 \\sim W1-C4 \\sim W1-C2 \\sim W1-C1 \\sim W1-C5
 with sigma of 0.02
 C9-C10 \\sim C9-C8 \\sim C8-C7 \\sim C6-C7 \\sim C10-C6
 with sigma of 0.02
 Ru1-C47 \\sim Ru1-C51 \\sim Ru1-C50 \\sim Ru1-C48 \\sim Ru1-C49
 with sigma of 0.02
 O3-C69 \\sim O2-C68 \\sim O1-C67
 with sigma of 0.02
 W1-C67 \\sim W1-C69 \\sim W1-C68
 with sigma of 0.02
3. Restrained planarity
 C5, C1, C2, C3, C4, C6, C8, C9, C7, C10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C5) = Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) =
Uanis(C6) = Uanis(C8) = Uanis(C10) = Uanis(C9) = Uanis(C62) = Uanis(C58) =
Uanis(C57) = Uanis(C61) = Uanis(C60) = Uanis(C59) = Uanis(C63) = Uanis(C66) =
Uanis(C64) = Uanis(C65)
Uanis(C7) = Uanis(C5) = Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) =
Uanis(C6) = Uanis(C8) = Uanis(C10) = Uanis(C9)
Uanis(C69) = Uanis(O3) = Uanis(O2) = Uanis(C68) = Uanis(C67) = Uanis(O1)
Uanis(C37) = Uanis(C38) = Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36)
Uanis(C21) = Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C23) = Uanis(C22)
Uanis(C50) = Uanis(C49) = Uanis(C48) = Uanis(C47) = Uanis(C55) = Uanis(C51) =
Uanis(C53) = Uanis(C54) = Uanis(C52) = Uanis(C56)
Uanis(C44) = Uanis(C43) = Uanis(C42) = Uanis(C41) = Uanis(C39) = Uanis(C40)
Uanis(C20) = Uanis(C19) = Uanis(C14) = Uanis(C16) = Uanis(C15) = Uanis(C18) =
Uanis(C17) = Uanis(C13) = Uanis(C12) = Uanis(C11)
Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C32)
5. Others
 Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C58)=Sof(C57)=Sof(C61)=Sof(C60)=
 Sof(C59)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C66)=Sof(H66A)=Sof(H66B)=
 Sof(H66C)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C65)=Sof(H65A)=Sof(H65B)=
 Sof(H65C)=1-FVAR(1)
 Sof(C7)=Sof(H01P)=Sof(H01Q)=Sof(H01R)=Sof(C5)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=
 Sof(C6)=Sof(H01S)=Sof(H01T)=Sof(H01U)=Sof(C8)=Sof(H01V)=Sof(H01W)=Sof(H01X)=
 Sof(C10)=Sof(H01Y)=Sof(H)=Sof(HA)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
6.a Free rotating group:
 C7(C5,C1,C2,C3,C4,C6,C8,C10,C9), C62(C58,C57,C61,C60,C59,C63,C66,C64,C65)
6.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C45(H45A,H45B)
6.c Me refined with riding coordinates:
 C7(H01P,H01Q,H01R), C6(H01S,H01T,H01U), C8(H01V,H01W,H01X), C10(H01Y,H,HA),
 C9(H9A,H9B,H9C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C66(H66A,H66B,H66C),
  C64(H64A,H64B,H64C), C65(H65A,H65B,H65C)
6.d Aromatic/amide H refined with riding coordinates:
 C44(H44), C43(H43), C42(H42), C41(H41), C40(H40), C17(H17), C18(H18),
 C14(H14), C15(H15), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C37(H37),
  C38(H38), C34(H34), C35(H35), C36(H36), C26(H26), C25(H25), C24(H24),
 C23(H23), C22(H22)
6.e Fitted hexagon refined as free rotating group:
 C39(C44,C43,C42,C41,C40), C16(C17,C18,C13,C14,C15), C27(C28,C29,C30,C31,C32),
 C37(C38,C33,C34,C35,C36), C21(C26,C25,C24,C23,C22)
6.f Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C52(H52A,H52B,
 H52C)
;
_shelx_res_checksum              48947
_shelx_hkl_checksum              13879
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.458
_oxdiff_exptl_absorpt_empirical_full_min 0.240