Iron vs. ruthenium: syntheses, structures and IR spectroelectrochemical characterisation of half-sandwich Group 8 acetylide complexes
Harrison, Daniel P.; Kumar, Varshini J.; Noppers, Johanna N.; Gluyas, Josef B. G.; Sobolev, Alexandre N.; Moggach, Stephen A.; Low, Paul J.; New Journal of Chemistry 45 (2021) 14932–14943; doi:10.1039/D0NJ03093G

data_7059881
_publ_section_title
;
 Iron vs. ruthenium: syntheses, structures and IR spectroelectrochemical
 characterisation of half-sandwich Group 8 acetylide complexes
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14932
_journal_page_last               14943
_journal_paper_doi               10.1039/D0NJ03093G
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H48 P2 Ru'
_chemical_formula_sum            'C42 H48 P2 Ru'
_chemical_formula_weight         715.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-06-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.473(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7348(2)
_cell_length_b                   19.3206(4)
_cell_length_c                   10.6426(2)
_cell_measurement_reflns_used    21893
_cell_measurement_temperature    99(3)
_cell_measurement_theta_max      27.3910
_cell_measurement_theta_min      3.5710
_cell_volume                     1784.61(6)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_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    -48.00  73.00   1.00    7.50    --  -11.48  77.00  30.00  121
  2  \w    -25.00  96.00   1.00    7.50    --   11.56  77.00 -60.00  121
  3  \w    -25.00  96.00   1.00    7.50    --   11.56  77.00  90.00  121
  4  \w    -25.00  96.00   1.00    7.50    --   11.56  77.00 150.00  121
  5  \w   -104.00 -35.00   1.00    7.50    --  -11.48-178.00-180.00   69
  6  \w   -104.00 -35.00   1.00    7.50    --  -11.48-178.00  60.00   69
  7  \w     -4.00  56.00   1.00    7.50    --   11.56 -99.00 120.00   60
  8  \w     -4.00  56.00   1.00    7.50    --   11.56 -99.00 -30.00   60
  9  \w    -66.00  44.00   1.00    7.50    --   11.56 -57.00-180.00  110
 10  \w     57.00 104.00   1.00    7.50    --   11.56 178.00 -30.00   47
 11  \w    -63.00  14.00   1.00    7.50    --  -11.48 112.00 153.00   77
 12  \w     -4.00  56.00   1.00    7.50    --   11.56 -99.00-180.00   60
 13  \w     57.00 104.00   1.00    7.50    --   11.56 178.00-120.00   47
 14  \w      8.00  63.00   1.00    7.50    --   11.56-112.00  61.00   55
 15  \w    -80.00  77.00   1.00    7.50    --   11.56   0.00-180.00  157
 16  \w     -4.00  56.00   1.00    7.50    --   11.56 -99.00 -90.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0780968000
_diffrn_orient_matrix_UB_12      -0.0107541000
_diffrn_orient_matrix_UB_13      -0.0050995000
_diffrn_orient_matrix_UB_21      -0.0239860000
_diffrn_orient_matrix_UB_22      0.0343936000
_diffrn_orient_matrix_UB_23      -0.0149984000
_diffrn_orient_matrix_UB_31      0.0021817000
_diffrn_orient_matrix_UB_32      -0.0070601000
_diffrn_orient_matrix_UB_33      -0.0651572000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            55220
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.218
_diffrn_reflns_theta_min         3.155
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 2997 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.047(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         8148
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0167P)^2^+1.2232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.884
_reflns_number_gt                7175
_reflns_number_total             8148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03093g2.cif
_cod_data_source_block           dph121
_cod_depositor_comments
'Adding full bibliography for 7059874--7059882.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7059881
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru1 P2 C36 H35'
_chemical_oxdiff_usercomment     'Varshini for P Low'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C35) = Uanis(C36) = Uanis(C37) = Uanis(C33) = Uanis(C34)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C16(H16), C10(H10), C28(H28), C14(H14), C17(H17), C25(H25),
 C24(H24), C12(H12), C30(H30), C18(H18), C29(H29), C11(H11), C20(H20), C19(H19),
  C23(H23), C13(H13), C22(H22), C32(H32), C31(H31)
3.c Idealised Me refined as rotating group:
 C340(H34A,H34B,H34C), C350(H35A,H35B,H35C), C330(H33A,H33B,H33C), C370(H37A,
 H37B,H37C), C360(H36A,H36B,H36C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C4(H4A,H4B,
 H4C)
;
_shelx_res_checksum              63993
_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 1.091
_oxdiff_exptl_absorpt_empirical_full_min 0.932