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_1549741
_publ_section_title
;
 Metal-ligand pair anisotropy in a series of mononuclear Er-COT complexes.
;
_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         'C12 H14 Er I N2'
_chemical_formula_sum            'C12 H14 Er I N2'
_chemical_formula_weight         480.41
_chemical_name_systematic
'(\h8-cyclooctatetraenyl)-bis(acetonitrile)-erbium-iodide '
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7394(11)
_cell_length_b                   10.7693(10)
_cell_length_c                   12.2067(12)
_cell_measurement_reflns_used    3980
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.52
_cell_volume                     1411.8(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10038
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         2.526
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.108
_exptl_absorpt_correction_T_max  0.4901
_exptl_absorpt_correction_T_min  0.3702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1170 before and 0.0571 after correction. The Ratio of minimum to maximum transmission is 0.7554. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.260
_exptl_crystal_description       plank
_exptl_crystal_F_000             884
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN'
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Flack x determined using 958 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0223
_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          0.0368
_refine_ls_wR_factor_ref         0.0378
_reflns_Friedel_coverage         0.726
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                2421
_reflns_number_total             2577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01361f2.cif
_cod_data_source_block           jr_100_0m
_cod_depositor_comments
'Adding full bibliography for 1549741--1549744.cif.'
_cod_database_code               1549741
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.519
_shelx_estimated_absorpt_t_min   0.297
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C6(H6), C3(H3), C5(H5), C2(H2), C4(H4), C7(H7), C1(H1)
2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              92667
_olex2_submission_special_instructions 'No special instructions were received'