Cyaphide-alkynyl complexes: metal-ligand conjugation and the influence of remote substituents.
Furfari, Samantha K.; Leech, Matthew C.; Trathen, Nicola; Levis, Madeleine C.; Crossley, Ian R.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8131–8143; doi:10.1039/c9dt01071h

data_7049835
_publ_section_title
;
 Cyaphide-alkynyl complexes: metal-ligand conjugation and the influence of
 remote substituents.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8131
_journal_page_last               8143
_journal_paper_doi               10.1039/c9dt01071h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C57 H51 O2 P5 Ru, 3.5(C6 H6)'
_chemical_formula_sum            'C78 H72 O2 P5 Ru'
_chemical_formula_weight         1297.27
_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             2019-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-15 deposited with the CCDC.    2019-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                82.979(4)
_cell_angle_beta                 81.078(4)
_cell_angle_gamma                67.587(5)
_cell_formula_units_Z            2
_cell_length_a                   10.3386(5)
_cell_length_b                   13.4556(8)
_cell_length_c                   26.1086(13)
_cell_measurement_reflns_used    8706
_cell_measurement_temperature    173
_cell_measurement_theta_max      70.9800
_cell_measurement_theta_min      4.6520
_cell_volume                     3309.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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     20.00 104.00   1.00    4.00    --   36.75  57.00 -60.00   84
  2  \w     39.00 117.00   1.00   36.00    --  107.00 -45.00   0.00   78
  3  \w     68.00 137.00   1.00   36.00    --  107.00 -90.00  48.30   69
  4  \w     68.00 127.00   1.00   36.00    --  107.00 -93.00 157.40   59
  5  \w     39.00 106.00   1.00   36.00    --  107.00 -45.00 120.00   67
  6  \w     38.00  64.00   1.00   36.00    --  107.00 -93.00 157.40   26
  7  \w    -30.00  63.00   1.00    4.00    --   36.75 -77.00  90.00   93
  8  \w     32.00  76.00   1.00    4.00    --   36.75 -99.00 -30.00   44
  9  \w     45.00 175.00   1.00   36.00    --  107.00   0.00-150.00  130
 10  \w    149.00 174.00   1.00   36.00    --  107.00  61.00 -90.00   25
 11  \w    108.00 134.00   1.00   36.00    --  107.00  61.00 -90.00   26
 12  \w     92.00 166.00   1.00   36.00    --  107.00  45.00-120.00   74
 13  \w     58.00 124.00   1.00   36.00    --  107.00 -45.00-180.00   66
 14  \w     50.00 133.00   1.00   36.00    --  107.00 -93.00 -63.22   83
 15  \w     41.00 121.00   1.00   36.00    --  107.00 -45.00 -90.00   80
 16  \w     10.00 101.00   1.00    4.00    --   36.75  77.00-150.00   91
 17  \w     40.00  66.00   1.00    4.00    --   36.75 178.00-120.00   26
 18  \w   -106.00 -19.00   1.00    4.00    --  -36.75 -38.00 -30.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0056139000
_diffrn_orient_matrix_UB_12      -0.1125507000
_diffrn_orient_matrix_UB_13      -0.0008777000
_diffrn_orient_matrix_UB_21      0.1490741000
_diffrn_orient_matrix_UB_22      -0.0521748000
_diffrn_orient_matrix_UB_23      0.0169102000
_diffrn_orient_matrix_UB_31      -0.0639913000
_diffrn_orient_matrix_UB_32      0.0047016000
_diffrn_orient_matrix_UB_33      0.0574272000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18582
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.846
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       prism
_exptl_crystal_F_000             1350
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.135
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         11729
_refine_ls_number_restraints     182
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0713P)^2^+5.9952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9839
_reflns_number_total             11729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01071h3.cif
_cod_data_source_block           ml03028
_cod_depositor_comments
'Adding full bibliography for 7049832--7049836.cif.'
_cod_database_code               7049835
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C57 H51 P5 O2 Ru1'
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid bond restraints
 O6, O6, C3AA, O6, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3BB, C8AB, C9AB, C0BB, C1BB, C2BB, O6A, O6A, C3AA, O6A, C8AB, C3BB, C3BB,
 C2BB, C9AB, C8AB, C2BB, C1BB, C9AB, C0BB, C1BB, C0BB
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5AB, C6AB, C7AB, C4A, C5A, C4AB, C7AB, C6AB, C6AB, C4A, C7AB, C5A, C4AB, C4A,
  C5AB, C5A, C5AB, C4AB
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9AB, C3BB, C8AB, C2BB, C1BB, C0BB, C8AB, C3BB, C3BB, C2BB, C9AB, C8AB, C2BB,
 C1BB, C9AB, C0BB, C1BB, C0BB
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C8AC, C9AC, C0BC, C1BC, C2BC, C3BC, C9AC, C8AC, C8AC, C3BC, C9AC, C0BC, C3BC,
 C2BC, C1BC, C0BC, C2BC, C1BC
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C0BB \\sim C3BB \\sim C8AB \\sim C2BB \\sim C9AB \\sim C1BB \\sim C8AB \\sim
C3BB \\sim C3BB \\sim C2BB \\sim C9AB \\sim C8AB \\sim C2BB \\sim C1BB \\sim
C9AB \\sim C0BB \\sim C1BB \\sim C0BB: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C5AB \\sim C6AB \\sim C7AB \\sim C4A \\sim C5A \\sim C4AB \\sim C7AB \\sim C6AB
\\sim C6AB \\sim C4A \\sim C7AB \\sim C5A \\sim C4AB \\sim C4A \\sim C5AB \\sim
C5A \\sim C5AB \\sim C4AB: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C3BB \\sim C8AB \\sim C9AB \\sim C0BB \\sim C1BB \\sim C2BB \\sim C8AB \\sim
C3BB \\sim C3BB \\sim C2BB \\sim C9AB \\sim C8AB \\sim C2BB \\sim C1BB \\sim
C9AB \\sim C0BB \\sim C1BB \\sim C0BB: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C8AC \\sim C9AC \\sim C3BC \\sim C0BC \\sim C2BC \\sim C1BC \\sim C9AC \\sim
C8AC \\sim C8AC \\sim C3BC \\sim C9AC \\sim C0BC \\sim C3BC \\sim C2BC \\sim
C1BC \\sim C0BC \\sim C2BC \\sim C1BC: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O6A)=1-FVAR(1)
 Sof(O6)=FVAR(1)
 Sof(C8AC)=Sof(H8AC)=Sof(C9AC)=Sof(H9AC)=Sof(C0BC)=Sof(H0BC)=Sof(C1BC)=
 Sof(H1BC)=Sof(C2BC)=Sof(H2BC)=Sof(C3BC)=Sof(H3BC)=1-FVAR(2)
 Sof(C3BB)=Sof(H3BB)=Sof(C8AB)=Sof(H8AB)=Sof(C9AB)=Sof(H9AB)=Sof(C0BB)=
 Sof(H0BB)=Sof(C1BB)=Sof(H1BB)=Sof(C2BB)=Sof(H2BB)=FVAR(2)
 Fixed Sof: C4(0.5) H4(0.5) C5(0.5) H5(0.5) C1A(0.5) H1A(0.5) C1B(0.5)
 H1B(0.5) C1C(0.5) H1C(0.5) C1D(0.5) H1D(0.5)
6.a Free rotating group:
 C4(C5,C1A,C1B,C1C,C1D)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B), C6(H6A,H6B)
6.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C39(H39), C38(H38),
 C37(H37), C36(H36), C35(H35), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
  C57(H57), C53(H53), C54(H54), C55(H55), C56(H56), C23(H23), C27(H27),
 C26(H26), C25(H25), C24(H24), C33(H33), C29(H29), C30(H30), C32(H32), C11(H11),
  C12(H12), C14(H14), C13(H13), C15(H15), C21(H21), C20(H20), C19(H19),
 C18(H18), C17(H17), C58(H58), C63(H63), C62(H62), C61(H61), C60(H60), C59(H59),
  C6AB(H6AB), C7AB(H7AB), C5A(H5A), C5AB(H5AB), C4AB(H4AB), C4A(H4A),
 C3BB(H3BB), C8AB(H8AB), C9AB(H9AB), C0BB(H0BB), C1BB(H1BB), C2BB(H2BB),
 C4AA(H4AA), C8AC(H8AC), C9AC(H9AC), C0BC(H0BC), C1BC(H1BC), C2BC(H2BC),
 C3BC(H3BC), C4(H4), C5(H5), C1A(H1A), C1B(H1B), C1C(H1C), C1D(H1D)
6.d Fitted hexagon refined as free rotating group:
 C58(C63,C62,C61,C60,C59), C6AB(C7AB,C5A,C5AB,C4AB,C4A), C3BB(C8AB,C9AB,C0BB,
 C1BB,C2BB), C8AC(C9AC,C0BC,C1BC,C2BC,C3BC)
6.e Idealised Me refined as rotating group:
 C5BA(H5BA,H5BB,H5BC)
;
_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 1.465
_oxdiff_exptl_absorpt_empirical_full_min 0.640