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_7037058
_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 O'
_chemical_formula_sum            'C30 H22 O'
_chemical_formula_weight         398.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-05-12
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-24 deposited with the CCDC.
2015-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.003(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9596(4)
_cell_length_b                   12.7252(5)
_cell_length_c                   13.7959(4)
_cell_measurement_reflns_used    4542
_cell_measurement_temperature    100.19(10)
_cell_measurement_theta_max      30.3540
_cell_measurement_theta_min      3.3990
_cell_volume                     2099.57(12)
_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)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.19(10)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_details
;
  1 omega  -69.00  -43.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467 -179.0000  -60.0000 26

  2 omega  -94.00  -64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467 -179.0000   90.0000 30

  3 omega  -19.00   20.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.9467  -99.0000 -120.0000 39

  4 omega    8.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   38.0000  -60.0000 83

  5 omega    5.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154   38.0000   30.0000 90

  6 omega  -50.00  -11.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4154  -38.0000  -90.0000 39
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0427224000
_diffrn_orient_matrix_UB_12      0.0087478000
_diffrn_orient_matrix_UB_13      -0.0347279000
_diffrn_orient_matrix_UB_21      0.0410897000
_diffrn_orient_matrix_UB_22      -0.0070149000
_diffrn_orient_matrix_UB_23      0.0364851000
_diffrn_orient_matrix_UB_31      0.0015581000
_diffrn_orient_matrix_UB_32      -0.0546290000
_diffrn_orient_matrix_UB_33      -0.0102282000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14157
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.596
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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)
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    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.7121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4892
_reflns_number_total             5809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03279b2.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
'Adding full bibliography for 7037058--7037062.cif.'
_cod_original_cell_volume        2099.57(13)
_cod_database_code               7037058
_chemical_oxdiff_formula         'N2 C40 H40'
_reflns_odcompleteness_completeness 99.80
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C15(H15), C25(H25), C27(H27), C20(H20), C12(H12), C26(H26),
 C14(H14), C19(H19), C29(H29), C23(H23), C24(H24), C9(H9), C28(H28), C10(H10),
 C8(H8), C5(H5), C13(H13), C11(H11), C4(H4)
;
_shelx_res_checksum              18925
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'