Molecular and electronic structures of donor-functionalized dysprosium pentadienyl complexes.
Day, Benjamin M.; Chilton, Nicholas F.; Layfield, Richard A.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7109–7113; doi:10.1039/c5dt00346f

data_7034268
_publ_section_title
;
 Molecular and electronic structures of donor-functionalized dysprosium
 pentadienyl complexes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7109
_journal_page_last               7113
_journal_paper_doi               10.1039/c5dt00346f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C24 H36 Dy N Si'
_chemical_formula_sum            'C24 H36 Dy N Si'
_chemical_formula_weight         529.13
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_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     direct
_audit_creation_date             2014-10-23
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Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
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_audit_update_record
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2015-01-23 deposited with the CCDC.
2015-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.103(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0020(5)
_cell_length_b                   23.8856(10)
_cell_length_c                   10.5417(6)
_cell_measurement_reflns_used    4545
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.6090
_cell_measurement_theta_min      3.3020
_cell_volume                     2333.4(2)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -24.00   19.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.0746  -99.0000 -180.0000 43

  2 omega  -70.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590  -57.0000 -120.0000 111

  3 omega  -14.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590  -99.0000    0.0000 83
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
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_diffrn_orient_matrix_UB_11      -0.0506144000
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_diffrn_orient_matrix_UB_13      0.0192041000
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_diffrn_orient_matrix_UB_22      -0.0247623000
_diffrn_orient_matrix_UB_23      0.0283939000
_diffrn_orient_matrix_UB_31      0.0550327000
_diffrn_orient_matrix_UB_32      0.0064425000
_diffrn_orient_matrix_UB_33      0.0640536000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9267
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       block
_exptl_crystal_F_000             1068
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.385
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0232P)^2^+0.5142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4082
_reflns_number_total             4772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00346f2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7034268--7034269.cif.'
_cod_database_code               7034268
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C50 H50 N1 Si1 Dy1'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C13(H13), C14(H14), C15(H15), C16(H16),
 C19(H19), C20(H20), C21(H21), C22(H22)
2.c X=CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              80937
_olex2_submission_special_instructions 'No special instructions were received'