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_7059878
_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_formula_moiety         'C40 H36 O P2 Ru'
_chemical_formula_sum            'C40 H36 O P2 Ru'
_chemical_formula_weight         695.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-06-14
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.3194(2)
_cell_length_b                   17.5662(4)
_cell_length_c                   39.2393(13)
_cell_measurement_reflns_used    3055
_cell_measurement_temperature    101.6(4)
_cell_measurement_theta_max      66.2420
_cell_measurement_theta_min      4.4910
_cell_volume                     6423.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      101.6(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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    -39.00  71.00   1.00   12.50    --   38.67 -57.00  90.00  110
  2  \w    -39.00  71.00   1.00   12.50    --   38.67 -57.00-180.00  110
  3  \w   -112.00  -9.00   1.00   15.00    --  -90.00 112.00 -90.00  103
  4  \w     12.00 133.00   1.00   15.00    --   96.50 -77.00-120.00  121
  5  \w     59.00 178.00   1.00   15.00    --   96.50  30.00-150.00  119
  6  \w     35.00 134.00   1.00   15.00    --   96.50 178.00   0.00   99
  7  \w     60.00 178.00   1.00   15.00    --   96.50  77.00 -60.00  118
  8  \w     10.00  84.00   1.00   15.00    --   96.50 -95.00  30.00   74
;
_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      -0.0058076000
_diffrn_orient_matrix_UB_12      -0.0852844000
_diffrn_orient_matrix_UB_13      0.0090313000
_diffrn_orient_matrix_UB_21      0.0056578000
_diffrn_orient_matrix_UB_22      0.0200491000
_diffrn_orient_matrix_UB_23      0.0381867000
_diffrn_orient_matrix_UB_31      -0.1651608000
_diffrn_orient_matrix_UB_32      0.0037639000
_diffrn_orient_matrix_UB_33      0.0009903000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            30269
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.333
_diffrn_reflns_theta_max         67.333
_diffrn_reflns_theta_min         4.507
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0255P)^2^+1.4838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3779
_reflns_number_total             5711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03093g2.cif
_cod_data_source_block           dph1-30_3
_cod_depositor_comments
'Adding full bibliography for 7059874--7059882.cif.'
_cod_database_code               7059878
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H36 O1 P2 Ru1'
_reflns_odcompleteness_completeness 99.54
_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.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C37(H37), C10(H10), C19(H19), C41(H41), C13(H13), C5(H5), C4(H4),
 C11(H11), C31(H31), C14(H14), C35(H35), C29(H29), C34(H34), C26(H26), C25(H25),
  C38(H38), C20(H20), C40(H40), C22(H22), C32(H32), C39(H39), C23(H23), C2(H2),
 C3(H3), C6(H6), C27(H27), C21(H21), C28(H28)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_shelx_res_checksum              35928
_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 1.235
_oxdiff_exptl_absorpt_empirical_full_min 0.859