Carbon-rich cyclopentadienyl ruthenium allenylidene complexes
Spörler, Susanne; Strinitz, Frank; Rodehutskors, Philipp; Müller, Lisa; Waterloo, Andreas R.; Dürr, Maximilian; Hübner, Eike; Ivanović-Burmazović, Ivana; Tykwinski, Rik R.; Burzlaff, Nicolai; New J. Chem. 40 (2016) 6127–; doi:10.1039/C5NJ03556B

data_7055547
_publ_section_title
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 Carbon-rich cyclopentadienyl ruthenium allenylidene complexes
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              6127
_journal_paper_doi               10.1039/C5NJ03556B
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C62 H45 P2 Ru, F6 P, C H2 Cl2'
_chemical_formula_sum            'C63 H47 Cl2 F6 P3 Ru'
_chemical_formula_weight         1182.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-06
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-06 deposited with the CCDC.
2016-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.389(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.6123(6)
_cell_length_b                   22.6218(6)
_cell_length_c                   25.5409(7)
_cell_measurement_reflns_used    16314
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.3010
_cell_measurement_theta_min      3.4320
_cell_volume                     11482.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -20.00   88.00   1.0000   59.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0947   77.0000  150.0000 108

  2 omega  -20.00   53.00   1.0000   59.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0947  -99.0000    0.0000 73

  3 omega  -20.00   53.00   1.0000   59.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0947  -99.0000 -180.0000 73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0022851000
_diffrn_orient_matrix_UB_12      -0.0057759000
_diffrn_orient_matrix_UB_13      -0.0277327000
_diffrn_orient_matrix_UB_21      -0.0057110000
_diffrn_orient_matrix_UB_22      0.0304812000
_diffrn_orient_matrix_UB_23      -0.0059879000
_diffrn_orient_matrix_UB_31      0.0351468000
_diffrn_orient_matrix_UB_32      0.0045987000
_diffrn_orient_matrix_UB_33      0.0049995000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            38940
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.350
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.889
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             4816
_exptl_crystal_size_max          0.3058
_exptl_crystal_size_mid          0.2526
_exptl_crystal_size_min          0.1162
_refine_diff_density_max         1.553
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0680P)^2^+47.9990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9065
_reflns_number_total             10493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03556b2.cif
_cod_data_source_block           buni150630
_cod_depositor_comments
'Adding full bibliography for 7055545--7055547.cif.'
_cod_database_code               7055547
_chemical_oxdiff_formula         'C H O Cl Ru P F'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.00
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Cl3(0.5) Cl4(0.5) C81(0.5) H81(0.5) H82(0.5) Cl1(0.5) C71(0.5)
 H72(0.5) H71(0.5) Cl2(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C81(H81,H82), C71(H72,H71)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C32(H32), C107(H107), C1AA(H1AA), C5(H5), C2(H2), C4(H4), C1(H1),
 C95(H95), C42(H42), C44(H44), C46(H46), C12(H12), C66(H66), C100(H100),
 C22(H22), C36(H36), C25(H25), C33(H33), C56(H56), C102(H102), C43(H43),
 C103(H103), C45(H45), C62(H62), C15(H15), C96(H96), C105(H105), C99(H99),
 C97(H97), C34(H34), C13(H13), C52(H52), C65(H65), C35(H35), C26(H26),
 C106(H106), C14(H14), C24(H24), C23(H23), C64(H64), C53(H53), C55(H55),
 C63(H63), C54(H54)
;
_shelx_res_checksum              66426
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-06-30
_olex2_submission_special_instructions 'No special instructions were received'