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_4348801
_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
'C30 H37 Cl Eu N8, Cl, 0.43(C0.99 H3.97 O), 0.57(C H3.99 O0.99), C O0.79'
_chemical_formula_sum            'C32 H41 Cl2 Eu N8 O1.79'
_chemical_formula_weight         789.27
_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'
_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                90
_cell_angle_beta                 107.542(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9432(8)
_cell_length_b                   14.6116(9)
_cell_length_c                   18.9914(11)
_cell_measurement_reflns_used    9197
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.31
_cell_measurement_theta_min      2.66
_cell_volume                     3424.6(4)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.1
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0263
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            116874
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.976
_diffrn_reflns_theta_min         1.650
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.028
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.5867
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0700 before and 0.0357 after correction.
The Ratio of minimum to maximum transmission is 0.7852.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1601
_refine_diff_density_max         3.547
_refine_diff_density_min         -2.036
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         15060
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0487P)^2^+10.4766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13038
_reflns_number_total             15060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01659_si_002.cif
_cod_data_source_block           Triphenyl_Aza222_EuCl2
_cod_database_code               4348801
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(C22) \\sim Ueq: with sigma of 0.0025 and sigma for terminal atoms of 0.005
3. Others
 Sof(O0)=Sof(H0)=1-FVAR(1)
 Sof(O2)=Sof(H2)=FVAR(1)
 Sof(C0AB)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=1-FVAR(2)
 Sof(C0AA)=Sof(H0AD)=Sof(H0AE)=Sof(H0AF)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 N4(H4)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
4.d Idealised Me refined as rotating group:
 C0AA(H0AD,H0AE,H0AF), C0AB(H0AA,H0AB,H0AC)
4.e Idealised tetrahedral OH refined as rotating group:
 O0(H0), O2(H2)
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_shelx_res_checksum              92289
_shelx_hkl_checksum              17
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'