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_7049834
_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         'C64 H61 F P5 Ru Si, F6 P, C H2 Cl2'
_chemical_formula_sum            'C65 H63 Cl2 F7 P6 Ru Si'
_chemical_formula_weight         1363.03
_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             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                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   13.4662(3)
_cell_length_b                   16.1621(4)
_cell_length_c                   28.4939(7)
_cell_measurement_reflns_used    15594
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.1820
_cell_measurement_theta_min      3.9930
_cell_volume                     6201.5(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 0.996
_diffrn_measured_fraction_theta_max 0.989
_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    -83.00   1.00   1.00   75.00    --  -15.97 -57.00 -90.00   84
  2  \w     -4.00  56.00   1.00   75.00    --   16.75 -99.00  30.00   60
  3  \w    -32.00  18.00   1.00   75.00    --   16.75 -38.00-180.00   50
  4  \w     20.00  46.00   1.00   75.00    --   16.75  57.00 -30.00   26
  5  \w    -51.00  43.00   1.00   75.00    --   16.75 -77.00-180.00   94
;
_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      -0.0268030000
_diffrn_orient_matrix_UB_12      0.0061239000
_diffrn_orient_matrix_UB_13      0.0211025000
_diffrn_orient_matrix_UB_21      0.0449508000
_diffrn_orient_matrix_UB_22      -0.0025091000
_diffrn_orient_matrix_UB_23      0.0129593000
_diffrn_orient_matrix_UB_31      0.0065125000
_diffrn_orient_matrix_UB_32      0.0433618000
_diffrn_orient_matrix_UB_33      -0.0022222000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            39263
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         3.355
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91851
_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    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             2792
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 5179 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         13451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0364P)^2^+3.1471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                12533
_reflns_number_total             13451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01071h3.cif
_cod_data_source_block           skf2071
_cod_depositor_comments
'Adding full bibliography for 7049832--7049836.cif.'
_cod_original_cell_volume        6201.4(3)
_cod_database_code               7049834
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C6H63Cl2F7P6RuSi
_cell_oxdiff_angle_alpha         90.011(2)
_cell_oxdiff_angle_beta          90.094(2)
_cell_oxdiff_angle_gamma         90.134(2)
_cell_oxdiff_length_a            13.4491(4)
_cell_oxdiff_length_b            16.1708(4)
_cell_oxdiff_length_c            28.5148(9)
_cell_oxdiff_measurement_reflns_used 15541
_cell_oxdiff_volume              6201.4(3)
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.803
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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), C39(H39A,H39B), C13(H13A,H13B), C14(H14A,H14B), C65(H65A,H65B)
2.b Aromatic/amide H refined with riding coordinates:
 C64(H64), C51(H51), C52(H52), C63(H63), C16(H16), C60(H60), C62(H62),
 C26(H26), C48(H48), C42(H42), C61(H61), C28(H28), C32(H32), C38(H38), C46(H46),
  C18(H18), C54(H54), C22(H22), C49(H49), C58(H58), C50(H50), C19(H19),
 C57(H57), C20(H20), C17(H17), C25(H25), C34(H34), C55(H55), C31(H31), C37(H37),
  C56(H56), C43(H43), C8(H8), C29(H29), C5(H5), C4(H4), C23(H23), C45(H45),
 C24(H24), C36(H36), C30(H30), C7(H7), C44(H44), C35(H35)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              43543
_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 1.101
_oxdiff_exptl_absorpt_empirical_full_min 0.859