Synthesis and electronic structure of the first cyaphide-alkynyl complexes.
Trathen, Nicola; Leech, Matthew C.; Crossley, Ian R.; Greenacre, Victoria K.; Roe, S. Mark; Dalton transactions (Cambridge, England : 2003) 43 (2014) 9004–9007; doi:10.1039/c4dt01108b

data_7030362
_publ_section_title
;
 Synthesis and electronic structure of the first cyaphide-alkynyl
 complexes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9004
_journal_page_last               9007
_journal_paper_doi               10.1039/c4dt01108b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C62 H55 O P5 Ru'
_chemical_formula_sum            'C62 H55 O P5 Ru'
_chemical_formula_weight         1071.98
_chemical_name_systematic
;
 ?
;
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4773)
;
_cell_angle_alpha                85.981(5)
_cell_angle_beta                 86.336(5)
_cell_angle_gamma                85.461(5)
_cell_formula_units_Z            2
_cell_length_a                   9.9951(7)
_cell_length_b                   11.9374(6)
_cell_length_c                   21.7684(13)
_cell_measurement_reflns_used    6430
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      70.9980
_cell_measurement_theta_min      3.6740
_cell_volume                     2578.3(3)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_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 0.984
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0569423000
_diffrn_orient_matrix_UB_12      -0.0940058000
_diffrn_orient_matrix_UB_13      0.0437813000
_diffrn_orient_matrix_UB_21      0.0354420000
_diffrn_orient_matrix_UB_22      -0.0850658000
_diffrn_orient_matrix_UB_23      -0.0496614000
_diffrn_orient_matrix_UB_31      0.1396082000
_diffrn_orient_matrix_UB_32      -0.0275401000
_diffrn_orient_matrix_UB_33      0.0258370000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14710
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.825
_diffrn_reflns_theta_min         3.722
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.252
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       needle
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.209
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         9644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0458
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7915
_reflns_number_total             9644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt01108b4.cif
_cod_data_source_block           ml_m_44b
_cod_depositor_comments
'Adding full bibliography for 7030361--7030363.cif.'
_cod_database_code               7030362
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         Ru1P5O1C62H55
_reflns_odcompleteness_completeness 98.57
_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
C10A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Others
 Fixed Sof: O1(0.5) C10A(0.5) H10A(0.5) H10B(0.5) H10C(0.5) O1A(0.5) C10(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C14(H14A,H14B), C12(H12A,H12B), C13(H13A,H13B)
4.b Aromatic/amide H refined with riding coordinates:
 C56(H56), C29(H29), C55(H55), C20(H20), C58(H58), C19(H19), C60(H60), C9(H9),
 C52(H52), C50(H50), C28(H28), C16(H16), C46(H46), C17(H17), C62(H62), C6(H6),
 C34(H34), C54(H54), C38(H38), C61(H61), C22(H22), C26(H26), C5(H5), C59(H59),
 C24(H24), C23(H23), C25(H25), C53(H53), C44(H44), C18(H18), C43(H43), C41(H41),
  C8(H8), C49(H49), C35(H35), C48(H48), C32(H32), C30(H30), C47(H47), C42(H42),
 C37(H37), C36(H36), C31(H31), C40(H40)
4.c Idealised Me refined as rotating group:
 C10A(H10A,H10B,H10C), C10(H10D,H10E,H10F)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'