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_7034269
_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         'C36 H76 Cl6 Dy2 Li2 N6 Si2'
_chemical_formula_sum            'C36 H76 Cl6 Dy2 Li2 N6 Si2'
_chemical_formula_weight         1200.78
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-01-23 deposited with the CCDC.
2015-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.080(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0325(3)
_cell_length_b                   16.3008(4)
_cell_length_c                   14.0042(4)
_cell_measurement_reflns_used    5727
_cell_measurement_temperature    150.04(13)
_cell_measurement_theta_max      28.2030
_cell_measurement_theta_min      3.1580
_cell_volume                     2746.29(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.04(13)
_diffrn_detector_area_resol_mean 10.3705
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -45.00   -4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6555   77.0000    0.0000 41

  2 omega  -67.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       11.6555    0.0000  150.0000 162
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0324849000
_diffrn_orient_matrix_UB_12      -0.0336487000
_diffrn_orient_matrix_UB_13      -0.0165103000
_diffrn_orient_matrix_UB_21      -0.0219860000
_diffrn_orient_matrix_UB_22      -0.0047959000
_diffrn_orient_matrix_UB_23      0.0463007000
_diffrn_orient_matrix_UB_31      -0.0440198000
_diffrn_orient_matrix_UB_32      0.0271702000
_diffrn_orient_matrix_UB_33      -0.0122352000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0848
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14094
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.892
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85026
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       plate
_exptl_crystal_F_000             1204
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5584
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0448
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4189
_reflns_number_total             5584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00346f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7034268--7034269.cif.'
_cod_database_code               7034269
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C20H20Cl2Dy1N1O1Si1
_reflns_odcompleteness_completeness 99.37
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-C18A \\sim N3-C18 \\sim N3-C17 \\sim N3-C17A
 with sigma of 0.02
 C16-N3 \\sim N3-C16A
 with sigma of 0.02
3. Rigid bond restraints
 C17A, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C18, C18A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16A, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C17 \\sim C17A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C18A \\sim C18: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
C16A \\sim C16: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
5. Others
 Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16C)=Sof(H16D)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(1)
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(2)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(3)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C15(H15A,H15B), C15(H15C,H15D), C16(H16A,H16B), C16A(H16C,H16D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
6.c X=CH2 refined with riding coordinates:
 C5(H5A,H5B)
6.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C18(H18A,H18B,H18C), C18A(H18D,H18E,
 H18F)
;
_shelx_res_checksum              19140
_olex2_submission_special_instructions 'No special instructions were received'