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_7049836
_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         '2(C63 H55 O2 P5 Ru), 2(C6 H6)'
_chemical_formula_sum            'C138 H122 O4 P10 Ru2'
_chemical_formula_weight         2356.37
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2019-03-07
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 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                110.850(4)
_cell_angle_beta                 90.296(4)
_cell_angle_gamma                93.812(4)
_cell_formula_units_Z            2
_cell_length_a                   9.2841(4)
_cell_length_b                   24.8606(11)
_cell_length_c                   26.8008(12)
_cell_measurement_reflns_used    7462
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.8910
_cell_measurement_theta_min      1.9030
_cell_volume                     5765.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9639
_diffrn_measured_fraction_theta_max 0.9639
_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    -88.00   8.00   1.00   10.00    --    0.00  52.00  30.00   96
  2  \w     28.00  78.00   1.00   10.00    --    0.00  52.00-120.00   50
  3  \w     25.00  89.00   1.00   10.00    --    0.00  52.00  30.00   64
  4  \w   -125.00 -78.00   1.00   47.50    --  -89.00  52.00 -60.00   47
  5  \w    -58.00 -19.00   1.00   47.50    --  -89.00  52.00-120.00   39
  6  \w    -56.00  -5.00   1.00   47.50    --  -89.00  52.00 -60.00   51
  7  \w   -177.00-148.00   1.00   47.50    --  -89.00  52.00 -60.00   29
  8  \w    -79.00 -29.00   1.00   47.50    --  -89.00   0.00-120.00   50
  9  \w   -170.00-133.00   1.00   47.50    --  -89.00  52.00-120.00   37
 10  \w   -126.00 -98.00   1.00   47.50    --  -89.00  52.00-120.00   28
 11  \w    -25.00   0.00   1.00   47.50    --  -89.00  52.00 150.00   25
 12  \w   -177.00 -26.00   1.00   47.50    --  -89.00  52.00  30.00  151
 13  \w   -177.00  -1.00   1.00   47.50    --  -89.00  52.00-180.00  176
 14  \w   -155.00-147.00   1.00   47.50    --  -89.00  52.00  60.00    8
 15  \w    -32.00 -18.00   1.00   47.50    --  -89.00  52.00  90.00   14
 16  \w   -165.00-140.00   1.00   47.50    --  -89.00  52.00  90.00   25
 17  \w   -131.00-100.00   1.00   47.50    --  -89.00  29.00  30.00   31
 18  \w   -165.00 -98.00   1.00   47.50    --  -89.00  52.00 -30.00   67
 19  \w    -84.00 -51.00   1.00   47.50    --  -89.00  52.00 -30.00   33
 20  \w   -164.00 -41.00   1.00   47.50    --  -89.00  52.00 -90.00  123
 21  \w   -157.00-119.00   1.00   47.50    --  -89.00  52.00 150.00   38
 22  \w   -104.00 -77.00   1.00   47.50    --  -89.00  52.00 150.00   27
 23  \w   -162.00-137.00   1.00   47.50    --  -89.00   0.00-120.00   25
 24  \w   -159.00-132.00   1.00   47.50    --  -89.00  52.00-150.00   27
 25  \w   -107.00 -80.00   1.00   47.50    --  -89.00  52.00-150.00   27
 26  \w    -59.00 -33.00   1.00   47.50    --  -89.00  52.00-150.00   26
 27  \w   -154.00-127.00   1.00   47.50    --  -89.00  52.00   0.00   27
 28  \w    -60.00 -33.00   1.00   47.50    --  -89.00  52.00   0.00   27
 29  \w    -80.00 -36.00   1.00   47.50    --  -89.00  52.00 120.00   44
 30  \w    -84.00 -57.00   1.00   47.50    --  -89.00  52.00  60.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1593656000
_diffrn_orient_matrix_UB_12      -0.0128568000
_diffrn_orient_matrix_UB_13      0.0025464000
_diffrn_orient_matrix_UB_21      0.0118291000
_diffrn_orient_matrix_UB_22      0.0400965000
_diffrn_orient_matrix_UB_23      0.0590862000
_diffrn_orient_matrix_UB_31      -0.0463220000
_diffrn_orient_matrix_UB_32      -0.0514557000
_diffrn_orient_matrix_UB_33      0.0170130000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1371
_diffrn_reflns_av_unetI/netI     0.1453
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62009
_diffrn_reflns_theta_full        67.0795
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         3.03
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.869
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
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    1.3573
_exptl_crystal_description       plate
_exptl_crystal_F_000             2451.9457
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         5.0245
_refine_diff_density_min         -1.1272
_refine_diff_density_rms         0.2486
_refine_ls_d_res_high            0.8370
_refine_ls_d_res_low             14.6028
_refine_ls_goodness_of_fit_ref   1.0374
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    234
_refine_ls_number_parameters     1365
_refine_ls_number_reflns         19809
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.0372
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.1013
_refine_ls_shift/su_max          0.1254
_refine_ls_shift/su_mean         0.0135
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1725P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2511
_refine_ls_wR_factor_ref         0.3048
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              27
_reflns_limit_k_min              -29
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                12314
_reflns_number_total             19809
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c9dt01071h3.cif
_cod_data_source_block           skf5025
_cod_depositor_comments
'Adding full bibliography for 7049832--7049836.cif.'
_cod_database_code               7049836
_chemical_oxdiff_formula         'Ru1 C100 H100 P5 O2'
_reflns_odcompleteness_completeness 96.41
_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. Uiso/Uaniso restraints and constraints
Uanis(C113) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C130, C132, H132, C131, C127, H131, C128, H127, C129, H130, H128, H129
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C135, C138, H138, C133, C137, C134, H133, C136, H137, H134, H136, H135
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C127, C132, C131, C129, C130, C128
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C114(H11d,H11e), C50(H50a,H50b), C87(H87a,H87b), C25(H25a,H25b), C88(H88a,
 H88b), C51(H51a,H51b), C24(H24a,H24b), C113(H11f,H11g)
4.b Aromatic/amide H refined with riding coordinates:
 C106(H106), C122(H122), C27(H27), C126(H126), C49(H49), C28(H28), C57(H57),
 C72(H72), C86(H86), C17(H17), C45(H45), C102(H102), C69(H69), C33(H33),
 C68(H68), C123(H123), C48(H48), C116(H116), C5(H5), C96(H96), C19(H19),
 C104(H104), C59(H59), C63(H63), C117(H117), C21(H21), C85(H85), C31(H31),
 C53(H53), C54(H54), C80(H80), C30(H30), C105(H105), C82(H82), C56(H56),
 C103(H103), C23(H23), C41(H41), C43(H43), C13(H13), C47(H47), C97(H97),
 C20(H20), C90(H90), C120(H120), C108(H108), C111(H111), C35(H35), C9(H9),
 C8(H8), C119(H119), C46(H46), C118(H118), C29(H29), C112(H112), C91(H91),
 C71(H71), C62(H62), C6(H6), C94(H94), C22(H22), C76(H76), C60(H60), C34(H34),
 C100(H100), C16(H16), C98(H98), C42(H42), C84(H84), C125(H125), C55(H55),
 C77(H77), C83(H83), C110(H110), C109(H109), C37(H37), C92(H92), C93(H93),
 C39(H39), C124(H124), C99(H99), C78(H78), C61(H61), C14(H14), C36(H36),
 C15(H15), C79(H79), C40(H40), C133(H133), C134(H134), C135(H135), C136(H136),
 C137(H137), C138(H138), C127(H127), C128(H128), C129(H129), C130(H130),
 C131(H131), C132(H132)
4.c Fitted hexagon refined as free rotating group:
 C133(C134,C135,C136,C137,C138), C127(C128,C129,C130,C131,C132)
4.d Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C74(H74a,H74b,H74c)
;
_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 4.515
_oxdiff_exptl_absorpt_empirical_full_min 0.437