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_1549744
_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         'C23 H30 B Er N6, C4 H8 O'
_chemical_formula_sum            'C27 H38 B Er N6 O'
_chemical_formula_weight         640.70
_chemical_name_systematic
'(\h8-cyclooctatetraenyl)-tris(3,5-dimethyl-1-pyrazolyl)borate erbium'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 102.020(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2903(12)
_cell_length_b                   31.840(5)
_cell_length_c                   10.584(3)
_cell_measurement_reflns_used    5296
_cell_measurement_temperature    200
_cell_measurement_theta_max      21.08
_cell_measurement_theta_min      2.34
_cell_volume                     2732.5(10)
_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 0.998
_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  0.0571
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28239
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.716
_diffrn_reflns_theta_max         24.716
_diffrn_reflns_theta_min         1.279
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.102
_exptl_absorpt_correction_T_max  0.4898
_exptl_absorpt_correction_T_min  0.4351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0627 before and 0.0498 after correction. The Ratio of minimum to maximum transmission is 0.8883. 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    1.557
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1292
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0318
_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^)+6.7769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3754
_reflns_number_total             4660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc01361f2.cif
_cod_data_source_block           jr_127_0m
_cod_depositor_comments
'Adding full bibliography for 1549741--1549744.cif.'
_cod_original_cell_volume        2732.5(9)
_cod_database_code               1549744
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.821
_shelx_estimated_absorpt_t_min   0.577
_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:
 C26(H26A,H26B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C21(H21), C5(H5), C16(H16), C7(H7), C11(H11), C8(H8), C4(H4), C1(H1A),
  C3(H3), C2(H2)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C19(H19A,H19B,
 H19C), C23(H23A,H23B,H23C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              5854
_olex2_submission_special_instructions 'No special instructions were received'