Unique Eu(II) Coordination Environments with a Janus Cryptand.
Jin, Guo-Xia; Bailey, Matthew D.; Allen, Matthew J.; Inorganic chemistry 55 (2016) 9085–9090; doi:10.1021/acs.inorgchem.6b01659

data_4348802
_publ_section_title
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 Unique Eu(II) Coordination Environments with a Janus Cryptand.
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_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9085
_journal_page_last               9090
_journal_paper_doi               10.1021/acs.inorgchem.6b01659
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'2(C30 H43 Eu N8 O2), 4(I), 2(C3 H6 O), 3.34(O)'
_chemical_formula_sum            'C66 H98 Eu2 I4 N16 O10'
_chemical_formula_weight         2087.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                88.736(6)
_cell_angle_beta                 74.793(5)
_cell_angle_gamma                78.543(5)
_cell_formula_units_Z            1
_cell_length_a                   10.5874(10)
_cell_length_b                   13.0022(13)
_cell_length_c                   15.2354(14)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.32
_cell_volume                     1982.5(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.1
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            74130
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.509
_diffrn_reflns_theta_min         1.386
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.187
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       cube
_exptl_crystal_F_000             1024
_refine_diff_density_max         5.035
_refine_diff_density_min         -4.049
_refine_diff_density_rms         0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         9306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0928
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1159P)^2^+67.9958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2544
_refine_ls_wR_factor_ref         0.2825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6752
_reflns_number_total             9306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01659_si_003.cif
_cod_data_source_block           Triphenyl_Aza222_EuI2
_cod_database_code               4348802
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C13)
Uanis(C24) = Uanis(C23)
3.a Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
3.b Ternary CH refined with riding coordinates:
 N8(H8), N6(H6), N4(H4)
3.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C30(H30A,H30B), C28(H28A,H28B), C19(H19A,H19B), C27(H27A,
 H27B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C23(H23A,H23B),
 C26(H26A,H26B), C29(H29A,H29B), C25(H25A,H25B)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C3(H3), C14(H14), C4(H4A), C8(H8A), C11(H11), C15(H15),
 C10(H10), C16(H16), C9(H9), C17(H17)
3.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              82505
_shelx_hkl_checksum              99714
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'