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_7232365
_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, 2.13(Br), 0.87(C F3 O3 S)'
_chemical_formula_sum            'C30.88 H53 Br2.12 Eu F2.62 N3 O21.62 S0.88'
_chemical_formula_weight         1211.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-03-26
_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                107.624(4)
_cell_angle_beta                 103.176(3)
_cell_angle_gamma                99.794(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5897(3)
_cell_length_b                   14.3802(7)
_cell_length_c                   18.8257(8)
_cell_measurement_reflns_used    8356
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.7660
_cell_measurement_theta_min      3.3160
_cell_volume                     2327.76(19)
_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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_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     13.00 116.00   1.00    1.50    --   41.90  77.00   0.00  103
  2  \w     79.00 175.00   1.00    3.00    --  112.00  77.00 120.00   96
  3  \w    129.00 178.00   1.00    3.00    --  112.00 111.00 150.00   49
  4  \w     57.00 151.00   1.00    3.00    --  112.00 178.00  30.00   94
  5  \w    114.00 176.00   1.00    3.00    --  112.00  61.00-120.00   62
  6  \w    104.00 167.00   1.00    3.00    --  112.00  61.00-150.00   63
  7  \w     87.00 178.00   1.00    3.00    --  112.00  45.00-180.00   91
  8  \w     73.00 116.00   1.00    3.00    --  112.00-111.00-150.00   43
  9  \w     40.00 116.00   1.00    3.00    --  112.00-111.00   0.00   76
 10  \w     48.00 133.00   1.00    3.00    --  112.00 -45.00 150.00   85
 11  \w     36.00 137.00   1.00    3.00    --  112.00 -77.00  60.00  101
 12  \w    -70.00  31.00   1.00    1.50    --  -41.90  57.00 150.00  101
 13  \w    -74.00  31.00   1.00    1.50    --  -41.90  77.00 -90.00  105
;
_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      0.0043345000
_diffrn_orient_matrix_UB_12      0.0768020000
_diffrn_orient_matrix_UB_13      -0.0419653000
_diffrn_orient_matrix_UB_21      0.1700673000
_diffrn_orient_matrix_UB_22      0.0207961000
_diffrn_orient_matrix_UB_23      0.0213057000
_diffrn_orient_matrix_UB_31      -0.0147197000
_diffrn_orient_matrix_UB_32      -0.0848691000
_diffrn_orient_matrix_UB_33      -0.0766391000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14473
_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         2.580
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.942
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.079
_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    1.729
_exptl_crystal_description       block
_exptl_crystal_F_000             1214
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.047
_refine_diff_density_max         2.214
_refine_diff_density_min         -1.972
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0937P)^2^+6.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8001
_reflns_number_total             8435
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_br_eu_otf_h2o_acet_red3
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        2327.76(18)
_cod_database_code               7232365
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12 S3 Br1 Eu1'
_chemical_oxdiff_usercomment     'clear colorless block'
_reflns_odcompleteness_completeness 99.37
_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. Others
 Sof(Br3B)=1-FVAR(1)
 Sof(S1A)=Sof(F8A)=Sof(F6A)=Sof(O4A)=Sof(O3A)=Sof(F7A)=Sof(O2A)=Sof(C5A)=FVAR(1)
3.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C10(H10A,H10B), C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C23(H23), C33(H33), C35(H35), C32(H32), C25(H25), C26(H26),
 C13(H13), C15(H15), C12(H12), C16(H16), C22(H22)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              73929
_shelx_fab_checksum              39164
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.723
_oxdiff_exptl_absorpt_empirical_full_min 0.574