Divalent ytterbium complexes with crown and heterocrown ethers.
Bartlett, Philip N.; Champion, Martin J. D.; Light, Mark E.; Levason, William; Reid, Gillian; Richardson, Peter W.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 2953–2955; doi:10.1039/c4dt03462g

data_7033281
_publ_section_title
;
 Divalent ytterbium complexes with crown and heterocrown ethers.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2953
_journal_page_last               2955
_journal_paper_doi               10.1039/c4dt03462g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C12 H24 I2 O4 Se2 Yb'
_chemical_formula_sum            'C12 H24 I2 O4 Se2 Yb'
_chemical_formula_weight         817.07
_chemical_name_common
di(Iodo)-(1,4,10,13-tetraoxa-7,16-diselena18-crown-6)-ytterbium(ii)
_chemical_name_systematic
di(Iodo)-(1,4,10,13-tetraoxa-7,16-diselenacyclooctadecane)-ytterbium(ii)
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-09-01
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-09-12 deposited with the CCDC.
2014-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.989(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.835(2)
_cell_length_b                   11.819(2)
_cell_length_c                   15.214(3)
_cell_measurement_reflns_used    2736
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.9
_cell_volume                     1945.6(6)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
scan:
    Number of images: 254
               Slice: -110.0000 - 17.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -60.0000
                 Phi: 0.0000
                 XTD: 44.8960
              2theta: -19.8261
scan:
    Number of images: 252
               Slice: -110.0000 - 16.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -70.0000
                 Phi: 225.0000
                 XTD: 44.8960
              2theta: -19.8261
scan:
    Number of images: 112
               Slice: -67.0000 - -11.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -70.0000
                 Phi: 135.0000
                 XTD: 44.8960
              2theta: -19.8261
scan:
    Number of images: 64
               Slice: -51.0000 - -19.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 45.0000
                 XTD: 44.8960
              2theta: -19.8261
scan:
    Number of images: 60
               Slice: 10.0000 - 40.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 0.0000
                 Phi: 135.0000
                 XTD: 44.8960
              2theta: -19.8261
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.037650
_diffrn_orient_matrix_UB_12      0.083014
_diffrn_orient_matrix_UB_13      0.015232
_diffrn_orient_matrix_UB_21      -0.075799
_diffrn_orient_matrix_UB_22      -0.030296
_diffrn_orient_matrix_UB_23      -0.022244
_diffrn_orient_matrix_UB_31      -0.013042
_diffrn_orient_matrix_UB_32      -0.013663
_diffrn_orient_matrix_UB_33      0.063051
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6782
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         2.552
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    11.731
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.789
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.485
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0607P)^2^+5.0964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2185
_reflns_number_total             2201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03462g2.cif
_cod_data_source_block           2014kmjdc99a1x_ml
_cod_depositor_comments          'Adding full bibliography for 7033281.cif.'
_cod_original_cell_volume        1945.7(6)
_cod_database_code               7033281
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.720
_shelx_estimated_absorpt_t_min   0.454
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B)
;
_shelx_res_checksum              92997
_olex2_submission_special_instructions 'No special instructions were received'