Diolefins with an ether/thioether functionality as ligands in the coordination sphere of Ni and Rh.
Lichtenberg, Crispin; Bloch, Jan; Gianetti, Thomas L.; Büttner, Torsten; Geier, Jens; Grützmacher, Hansjörg; Dalton transactions (Cambridge, England : 2003) 44 (2015) 20056–20066; doi:10.1039/c5dt03279b

data_7037059
_publ_section_title
;
 Diolefins with an ether/thioether functionality as ligands in the
 coordination sphere of Ni and Rh.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              20056
_journal_page_last               20066
_journal_paper_doi               10.1039/c5dt03279b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C30 H22 S'
_chemical_formula_sum            'C30 H22 S'
_chemical_formula_weight         414.53
_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     direct
_audit_creation_date             2015-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-24 deposited with the CCDC.
2015-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                81.261(2)
_cell_angle_beta                 88.908(3)
_cell_angle_gamma                66.905(3)
_cell_formula_units_Z            4
_cell_length_a                   10.2096(4)
_cell_length_b                   10.4182(3)
_cell_length_c                   22.8395(7)
_cell_measurement_reflns_used    11643
_cell_measurement_temperature    106.06(10)
_cell_measurement_theta_max      30.4780
_cell_measurement_theta_min      3.1810
_cell_volume                     2206.50(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      106.06(10)
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_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_details
;
  1 omega  -25.00    9.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000   90.0000 34

  2 omega    5.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904   57.0000  -60.0000 42

  3 omega  -91.00  -18.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -57.0000  150.0000 73

  4 omega  -42.00   23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904   57.0000   30.0000 65

  5 omega  -23.00   20.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000 -150.0000 43

  6 omega  -23.00   19.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -99.0000  -90.0000 42

  7 omega  -60.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904   19.0000  -60.0000 103

  8 omega   55.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2592  179.0000 -180.0000 40

  9 omega  -43.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904   57.0000   60.0000 90

 10 omega  -76.00  -30.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  120.0000 -177.0000 46

 11 omega  -95.00   22.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.7904  -19.0000 -120.0000 117
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0440420000
_diffrn_orient_matrix_UB_12      0.0198468000
_diffrn_orient_matrix_UB_13      0.0242135000
_diffrn_orient_matrix_UB_21      -0.0609749000
_diffrn_orient_matrix_UB_22      0.0304623000
_diffrn_orient_matrix_UB_23      -0.0197057000
_diffrn_orient_matrix_UB_31      -0.0076156000
_diffrn_orient_matrix_UB_32      -0.0655355000
_diffrn_orient_matrix_UB_33      0.0038227000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34948
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.721
_diffrn_reflns_theta_min         2.886
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         12267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0670P)^2^+1.0270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10446
_reflns_number_total             12267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03279b2.cif
_cod_data_source_block           Compound3
_cod_depositor_comments
'Adding full bibliography for 7037058--7037062.cif.'
_cod_original_cell_volume        2206.51(13)
_cod_database_code               7037059
_chemical_oxdiff_formula         C40H40S1
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C16(H16), C31(H31), C46(H46)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C19(H19), C11(H11), C23(H23), C20(H20), C4(H4), C30(H30),
 C26(H26), C27(H27), C9(H9), C10(H10), C29(H29), C24(H24), C15(H15), C12(H12),
 C25(H25), C13(H13), C28(H28), C14(H14), C49(H49), C50(H50), C53(H53), C56(H56),
  C60(H60), C38(H38), C34(H34), C45(H45), C35(H35), C55(H55), C54(H54),
 C41(H41), C57(H57), C58(H58), C42(H42), C43(H43), C39(H39), C40(H40), C59(H59),
  C44(H44)
;
_shelx_res_checksum              23044
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'