Metal-ligand pair anisotropy in a series of mononuclear Er-COT complexes.
Hilgar, J. D.; Bernbeck, M. G.; Flores, B. S.; Rinehart, J. D.; Chemical science 9 (2018) 7204–7209; doi:10.1039/c8sc01361f

data_1549742
_publ_section_title
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 Metal-ligand pair anisotropy in a series of mononuclear Er-COT complexes.
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_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              7204
_journal_page_last               7209
_journal_paper_doi               10.1039/c8sc01361f
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C16 H24 Er I O2'
_chemical_formula_sum            'C16 H24 Er I O2'
_chemical_formula_weight         542.51
_chemical_name_systematic
'(\h8-cyclooctatetraenyl)-bis(tetrahydrofuran)-erbium-iodide '
_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     dual
_audit_creation_date             2018-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-21 deposited with the CCDC.
2018-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.496(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4793(7)
_cell_length_b                   9.3962(7)
_cell_length_c                   22.2154(17)
_cell_measurement_reflns_used    5509
_cell_measurement_temperature    230
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.36
_cell_volume                     1754.8(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      230
_diffrn_detector_area_resol_mean 8.0
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13238
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.324
_diffrn_reflns_theta_min         1.849
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.541
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0676 before and 0.0368 after correction. The Ratio of minimum to maximum transmission is 0.8647. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_description       plank
_exptl_crystal_F_000             1028
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3202
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+5.2947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2767
_reflns_number_total             3202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01361f2.cif
_cod_data_source_block           jr_133_230_0m
_cod_depositor_comments
'Adding full bibliography for 1549741--1549744.cif.'
_cod_database_code               1549742
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.613
_shelx_estimated_absorpt_t_min   0.404
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 Er1-I1 \\sim Er1-I2
 with sigma of 0.01
 C15-C16 \\sim C14-C16 \\sim C16-C17 \\sim C17-C18 \\sim C12-C11 \\sim C13-C11
\\sim C11-C10 \\sim C10-C9
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C14) = Uanis(C15)
Uanis(I1) = Uanis(I2)
Uanis(C12) = Uanis(C13)
4. Others
 Sof(H16C)=Sof(H16D)=Sof(C15)=Sof(H15A)=Sof(H15B)=1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(C14)=Sof(H14A)=Sof(H14B)=FVAR(1)
 Sof(I1)=1-FVAR(2)
 Sof(I2)=FVAR(2)
 Sof(H11C)=Sof(H11D)=Sof(C13)=Sof(H13A)=Sof(H13B)=1-FVAR(3)
 Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C9(H9A,H9B), C17(H17A,H17B), C10(H10A,H10B), C16(H16C,H16D),
 C16(H16A,H16B), C11(H11C,H11D), C11(H11A,H11B), C15(H15A,H15B), C14(H14A,H14B),
  C13(H13A,H13B), C12(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C6(H6), C8(H8), C3(H3), C1(H1), C2(H2), C5(H5)
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_shelx_res_checksum              9480
_olex2_submission_special_instructions 'No special instructions were received'