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_7049832
_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         'C65 H64 P5 Ru Si, F6 P, C H2 Cl2'
_chemical_formula_sum            'C66 H66 Cl2 F6 P6 Ru Si'
_chemical_formula_weight         1359.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-14
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5338(4)
_cell_length_b                   16.2852(4)
_cell_length_c                   28.7574(8)
_cell_measurement_reflns_used    6431
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.1300
_cell_measurement_theta_min      4.0910
_cell_volume                     6338.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.44a (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      173.15
_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 0.971
_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     35.00 109.00   1.00   50.00    --   36.88 178.00-120.00   74
  2  \w     18.00 106.00   1.00   50.00    --   36.88  38.00 -30.00   88
  3  \w     89.00 174.00   1.00  220.00    --  107.00  61.00  90.00   85
  4  \w     41.00  84.00   1.00  220.00    --  107.00 -95.00-150.00   43
  5  \w     38.00  78.00   1.00  220.00    --  107.00 -95.00  60.00   40
  6  \w     44.00  87.00   1.00  220.00    --  107.00 -45.00-180.00   43
  7  \w     79.00 144.00   1.00  220.00    --  107.00 111.00 -60.00   65
;
_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      -0.0441246000
_diffrn_orient_matrix_UB_12      0.0114498000
_diffrn_orient_matrix_UB_13      -0.0489319000
_diffrn_orient_matrix_UB_21      -0.0017184000
_diffrn_orient_matrix_UB_22      0.0937691000
_diffrn_orient_matrix_UB_23      0.0074434000
_diffrn_orient_matrix_UB_31      0.1048097000
_diffrn_orient_matrix_UB_32      0.0062754000
_diffrn_orient_matrix_UB_33      -0.0205371000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13496
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.267
_diffrn_reflns_theta_min         3.609
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.872
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.44a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.571
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 2716 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         10598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0934P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1763
_reflns_Friedel_coverage         0.613
_reflns_Friedel_fraction_full    0.770
_reflns_Friedel_fraction_max     0.729
_reflns_number_gt                8576
_reflns_number_total             10598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01071h3.cif
_cod_data_source_block           skf_2070
_cod_depositor_comments
'Adding full bibliography for 7049832--7049836.cif.'
_cod_database_code               7049832
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C66H65Si1P6F6Ru1
_reflns_odcompleteness_completeness 99.11
_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.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B), C14(H14A,H14B), C15(H15A,H15B), C66(H66A,H66B)
2.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C47(H47), C58(H58), C59(H59), C55(H55), C46(H46), C61(H61),
 C65(H65), C56(H56), C49(H49), C20(H20), C53(H53), C17(H17), C57(H57), C39(H39),
  C29(H29), C24(H24), C62(H62), C31(H31), C50(H50), C18(H18), C38(H38),
 C23(H23), C36(H36), C44(H44), C45(H45), C37(H37), C8(H8), C52(H52), C43(H43),
 C35(H35), C51(H51), C64(H64), C63(H63), C30(H30), C25(H25), C33(H33), C7(H7),
 C32(H32), C19(H19), C4(H4), C27(H27), C26(H26), C5(H5)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              52262
_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 1.744
_oxdiff_exptl_absorpt_empirical_full_min 0.777