In-depth structural analysis of lanthanoid coordination networks based on a flexible tripodal zwitterionic isonicotinate ligand
Tiihonen, Antti; Lahtinen, Manu; CrystEngComm 21 (2019) 2286–; doi:10.1039/C8CE01015C

data_7232381
_publ_section_title
;
 In-depth structural analysis of lanthanoid coordination networks based on
 a flexible tripodal zwitterionic isonicotinate ligand
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2286
_journal_paper_doi               10.1039/C8CE01015C
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety
'C30 H31 Eu N3 O8, 1.55(C F3 O3 S), 1.45(Br), 0.45(O)'
_chemical_formula_sum            'C31.55 H43 Br1.45 Eu F4.64 N3 O19.1 S1.55'
_chemical_formula_weight         1175.63
_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     iterative
_audit_creation_date             2018-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-29 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.421(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6774(6)
_cell_length_b                   25.6718(7)
_cell_length_c                   9.7560(3)
_cell_measurement_reflns_used    4818
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.6530
_cell_measurement_theta_min      4.1870
_cell_volume                     4568.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -117.00 -11.00   1.00   12.50    --  -41.40 -77.00-120.00  106
  2  \w    -32.00  68.00   1.00   12.50    --   41.40 -19.00  60.00  100
  3  \w     44.00  88.00   1.00   70.00    --  112.00 -30.00-150.00   44
  4  \w     50.00  89.00   1.00   70.00    --  112.00 -30.00 -60.00   39
  5  \w    102.00 175.00   1.00   70.00    --  112.00 111.00  30.00   73
  6  \w     98.00 177.00   1.00   70.00    --  112.00  30.00 -30.00   79
  7  \w     38.00 143.00   1.00   70.00    --  112.00 -77.00  30.00  105
  8  \w     45.00  98.00   1.00   70.00    --  112.00 -45.00 -90.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0830577000
_diffrn_orient_matrix_UB_12      -0.0056889000
_diffrn_orient_matrix_UB_13      -0.0092795000
_diffrn_orient_matrix_UB_21      -0.0154113000
_diffrn_orient_matrix_UB_22      0.0369971000
_diffrn_orient_matrix_UB_23      -0.1272646000
_diffrn_orient_matrix_UB_31      -0.0021569000
_diffrn_orient_matrix_UB_32      -0.0469015000
_diffrn_orient_matrix_UB_33      -0.0992229000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0870
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14324
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.998
_diffrn_reflns_theta_min         2.972
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.813
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       plate
_exptl_crystal_F_000             2346
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.014
_refine_diff_density_max         1.936
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8271
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0835
_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^)+(0.1396P)^2^+20.6764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2359
_refine_ls_wR_factor_ref         0.2492
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6299
_reflns_number_total             8271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003-01-eu-otf-h2o_red4
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_formula_sum        'C31.55 H43 Br1.45 Eu F4.64 N3 O19.10 S1.55'
_cod_database_code               7232381
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C21 H20 O6 N3 F6 Eu'
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Restrained distances
 H1WA-Br1
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O39) = Uanis(O38) = Uanis(C37)
Uanis(O18) = Uanis(C17) = Uanis(O19)
4. Others
 Sof(Br2B)=Sof(O3B)=1-FVAR(1)
 Sof(O51A)=Sof(F53A)=Sof(O50A)=Sof(F54A)=Sof(F55A)=Sof(O49A)=Sof(C52A)=
 Sof(S48A)=FVAR(1)
5.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C10(H10A,H10B), C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C13(H13), C15(H15), C32(H32), C23(H23), C35(H35),
 C33(H33), C26(H26), C22(H22), C36(H36), C25(H25)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              1737
_shelx_fab_checksum              16849
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.529
_oxdiff_exptl_absorpt_empirical_full_min 0.657