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_7049833
_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         'C61 H52 F P5 Ru, 2(C6 H6)'
_chemical_formula_sum            'C73 H64 F P5 Ru'
_chemical_formula_weight         1216.16
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-10 deposited with the CCDC.    2019-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                98.356(3)
_cell_angle_beta                 93.032(3)
_cell_angle_gamma                104.248(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1652(5)
_cell_length_b                   15.8226(6)
_cell_length_c                   17.5577(5)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.1620
_cell_measurement_theta_min      4.0710
_cell_volume                     2961.7(2)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -95.00 -58.00   1.00    7.50    --  -36.88-178.00 -60.00   37
  2  \w   -104.00 -77.00   1.00    7.50    --  -36.88-178.00 150.00   27
  3  \w     10.00  97.00   1.00    7.50    --   36.88  77.00  90.00   87
  4  \w     58.00 104.00   1.00    7.50    --   36.88  57.00   0.00   46
  5  \w    -19.00  75.00   1.00    7.50    --   36.88 -99.00-180.00   94
  6  \w    -25.00  76.00   1.00    7.50    --   36.88 -99.00 -30.00  101
  7  \w    -34.00  45.00   1.00    7.50    --   36.88 -19.00-180.00   79
  8  \w     39.00 173.00   1.00   25.00    --  107.00   0.00 -30.00  134
  9  \w     89.00 116.00   1.00   25.00    --  107.00 -93.00 -25.47   27
 10  \w     77.00 139.00   1.00   25.00    --  107.00 -93.00-115.47   62
 11  \w     46.00 124.00   1.00   25.00    --  107.00 -45.00 150.00   78
 12  \w     39.00 124.00   1.00   25.00    --  107.00 -45.00  30.00   85
 13  \w     39.00 116.00   1.00   25.00    --  107.00 -45.00-120.00   77
 14  \w     43.00 114.00   1.00   25.00    --  107.00 -30.00 -60.00   71
 15  \w     74.00 131.00   1.00   25.00    --  107.00 -91.00 169.89   57
 16  \w    101.00 170.00   1.00   25.00    --  107.00  30.00-180.00   69
 17  \w     90.00 116.00   1.00   25.00    --  107.00  61.00-180.00   26
 18  \w     39.00  71.00   1.00   25.00    --  107.00 -91.00 169.89   32
 19  \w     42.00 106.00   1.00   25.00    --  107.00 -92.00  35.43   64
 20  \w    106.00 133.00   1.00   25.00    --  107.00  61.00-150.00   27
 21  \w     75.00 139.00   1.00   25.00    --  107.00 -93.00  85.43   64
;
_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      0.0682770000
_diffrn_orient_matrix_UB_12      0.0843378000
_diffrn_orient_matrix_UB_13      -0.0295473000
_diffrn_orient_matrix_UB_21      -0.1158632000
_diffrn_orient_matrix_UB_22      0.0359709000
_diffrn_orient_matrix_UB_23      0.0074739000
_diffrn_orient_matrix_UB_31      0.0485201000
_diffrn_orient_matrix_UB_32      0.0442918000
_diffrn_orient_matrix_UB_33      0.0836884000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18469
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.074
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         4.103
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72286
_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            'light yellow'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       plate
_exptl_crystal_F_000             1260
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         10532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0485P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8756
_reflns_number_total             10532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01071h3.cif
_cod_data_source_block           skf_3081
_cod_depositor_comments
'Adding full bibliography for 7049832--7049836.cif.'
_cod_database_code               7049833
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C142 H128 F4 P12 Ru2 '
_reflns_odcompleteness_completeness 99.68
_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
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C11(H11A,H11B), C10(H10A,H10B), C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C45(H45), C13(H13), C19(H19), C39(H39), C29(H29), C43(H43),
 C31(H31), C34(H34), C42(H42), C17(H17), C49(H49), C61(H61), C33(H33), C51(H51),
  C27(H27), C9(H9), C32(H32), C55(H55), C21(H21), C57(H57), C20(H20), C5(H5),
 C28(H28), C46(H46), C15(H15), C58(H58), C26(H26), C22(H22), C66(H66), C8(H8),
 C25(H25), C67(H67), C54(H54), C47(H47), C40(H40), C48(H48), C65(H65), C41(H41),
  C23(H23), C14(H14), C53(H53), C60(H60), C62(H62), C16(H16), C64(H64),
 C72(H72), C52(H52), C73(H73), C6(H6), C68(H68), C59(H59), C71(H71), C69(H69),
 C63(H63), C70(H70)
;
_shelx_res_checksum              53929
_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 2.235
_oxdiff_exptl_absorpt_empirical_full_min 0.569