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_7232384
_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         'C32 H30 N3 Nd O8, 2(Br), 7(H2 O)'
_chemical_formula_sum            'C32 H44 Br2 N3 Nd O15'
_chemical_formula_weight         1014.76
_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             2019-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-31 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                106.661(7)
_cell_angle_beta                 100.429(7)
_cell_angle_gamma                91.716(8)
_cell_formula_units_Z            2
_cell_length_a                   8.7309(9)
_cell_length_b                   12.2707(11)
_cell_length_c                   19.3079(11)
_cell_measurement_reflns_used    6499
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.5370
_cell_measurement_theta_min      3.7280
_cell_volume                     1941.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.996
_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   -115.00 -17.00   2.00    3.00    --  -41.78 -37.00 120.00   49
  2  \w    -54.00  -2.00   2.00    3.00    --  -41.78 125.00   0.00   26
  3  \w    -66.00  24.00   2.00    3.00    --  -41.78  37.00 -60.00   45
  4  \w      1.00  71.00   2.00    3.00    --   41.78 -99.00   0.00   35
  5  \w     38.00  98.00   2.00    3.00    --   41.78-125.00-180.00   30
  6  \w     72.00 176.00   2.00    6.00    --  112.00  15.00-120.00   52
  7  \w    146.00 178.00   2.00    6.00    --  112.00 111.00  60.00   16
  8  \w     38.00 118.00   2.00    6.00    --  112.00 -30.00-150.00   40
  9  \w    101.00 129.00   2.00    6.00    --  112.00 111.00  60.00   14
 10  \w     50.00 116.00   2.00    6.00    --  112.00-111.00 120.00   33
 11  \w     36.00 116.00   2.00    6.00    --  112.00-111.00 -90.00   40
 12  \w     84.00 178.00   2.00    6.00    --  112.00  30.00 150.00   47
 13  \w     77.00 103.00   2.00    6.00    --  112.00 -94.00-180.00   13
 14  \w     33.00 109.00   2.00    6.00    --  112.00 -94.00   0.00   38
 15  \w     41.00 137.00   2.00    6.00    --  112.00 -45.00 -30.00   48
 16  \w     49.00 139.00   2.00    6.00    --  112.00 -61.00  90.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0341239000
_diffrn_orient_matrix_UB_12      0.1285673000
_diffrn_orient_matrix_UB_13      0.0115588000
_diffrn_orient_matrix_UB_21      -0.1721524000
_diffrn_orient_matrix_UB_22      0.0184291000
_diffrn_orient_matrix_UB_23      0.0044246000
_diffrn_orient_matrix_UB_31      0.0404110000
_diffrn_orient_matrix_UB_32      0.0208641000
_diffrn_orient_matrix_UB_33      0.0840614000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12498
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.991
_diffrn_reflns_theta_min         3.774
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.225
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.298
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
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    1.736
_exptl_crystal_description       block
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         7055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0277P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6658
_reflns_number_total             7055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_ndoac_dry_h2o_acet_red2
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_database_code               7232384
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C32 H30 N3 O18 Nd1 Br2'
_shelx_estimated_absorpt_t_max   0.558
_shelx_estimated_absorpt_t_min   0.240
_reflns_odcompleteness_completeness 99.46
_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.a Free rotating group:
 O6W(H6WA,H6WB), O1W(H1WA,H1WB), O7W(H7WA,H7WB), O2W(H2WA,H2WB), O4W(H4WA,
 H4WB), O0AA(H0AA,H0AB), O5W(H5WA,H5WB)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C10(H10A,H10B), C20(H20A,H20B)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C35(H35), C13(H13), C16(H16), C26(H26), C33(H33), C22(H22),
 C25(H25), C15(H15), C12(H12), C36(H36), C32(H32)
2.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              50488
_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 1.183
_oxdiff_exptl_absorpt_empirical_full_min 0.819