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_7232372
_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 N3 Nd O8, 1.35(Br), 1.65(C F3 O3 S), 0.35(O)'
_chemical_formula_sum            'C31.65 H43 Br1.35 F4.94 N3 Nd O19.29 S1.65'
_chemical_formula_weight         1173.14
_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             2018-03-26
_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                90
_cell_angle_beta                 102.8557(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7643(2)
_cell_length_b                   25.6962(3)
_cell_length_c                   9.85675(12)
_cell_measurement_reflns_used    7481
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.5540
_cell_measurement_theta_min      4.1810
_cell_volume                     4633.51(10)
_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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -118.00  -9.00   1.00   20.00    --  -42.03 -77.00  90.00  109
  2  \w    -70.00  30.00   1.00   20.00    --  -42.03  57.00 -30.00  100
  3  \w    104.00 178.00   1.00   60.00    --  112.00 111.00   0.00   74
  4  \w     84.00 178.00   1.00   60.00    --  112.00  30.00   0.00   94
  5  \w     43.00 111.00   1.00   60.00    --  112.00-111.00 -60.00   68
  6  \w    104.00 143.00   1.00   60.00    --  112.00 111.00-150.00   39
  7  \w     33.00 105.00   1.00   60.00    --  112.00 -94.00  90.00   72
  8  \w     39.00 131.00   1.00   60.00    --  112.00 -45.00  60.00   92
;
_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      0.0477035000
_diffrn_orient_matrix_UB_12      -0.0490615000
_diffrn_orient_matrix_UB_13      0.0352766000
_diffrn_orient_matrix_UB_21      0.0675415000
_diffrn_orient_matrix_UB_22      0.0344363000
_diffrn_orient_matrix_UB_23      0.0545311000
_diffrn_orient_matrix_UB_31      -0.0161690000
_diffrn_orient_matrix_UB_32      -0.0009329000
_diffrn_orient_matrix_UB_33      0.1464746000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.994
_diffrn_reflns_theta_min         2.965
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.453
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.539
_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    1.682
_exptl_crystal_description       block
_exptl_crystal_F_000             2346
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.088
_refine_diff_density_min         -1.910
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         8412
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0792P)^2^+8.8951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6956
_reflns_number_total             8412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_br_nd_otf_kotf_ii_h2o_acet_red2
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        4633.50(10)
_cod_database_code               7232372
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C32 H31 Br1 F5 N3 Nd1 O13 S2'
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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. Uiso/Uaniso restraints and constraints
Uanis(O3B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(Br2B)=Sof(O3B)=1-FVAR(1)
 Sof(S48A)=Sof(O50A)=Sof(O49A)=Sof(O51A)=Sof(F53A)=Sof(F55A)=Sof(F54A)=
 Sof(C52A)=FVAR(1)
4.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C30(H30A,H30B)
4.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C12(H12), C23(H23), C26(H26), C13(H13), C22(H22),
 C25(H25), C35(H35), C36(H36), C32(H32), C33(H33)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              65796
_shelx_fab_checksum              69948
_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 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.889