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_7232385
_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, 3(N O3), O'
_chemical_formula_sum            'C30 H43 N6 Nd O23'
_chemical_formula_weight         999.94
_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             2018-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-09 deposited with the CCDC.    2019-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                106.033(6)
_cell_angle_beta                 99.619(6)
_cell_angle_gamma                99.928(6)
_cell_formula_units_Z            2
_cell_length_a                   9.5948(6)
_cell_length_b                   12.3229(9)
_cell_length_c                   18.8983(13)
_cell_measurement_reflns_used    8244
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      75.9390
_cell_measurement_theta_min      3.7810
_cell_volume                     2060.3(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      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_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    -67.00  31.00   2.00    2.00    --  -41.78  70.00 -89.00   49
  2  \w   -107.00 -13.00   2.00    2.00    --  -41.78 -77.00 150.00   47
  3  \w    -74.00  34.00   2.00    2.00    --  -41.78  77.00  30.00   54
  4  \w     47.00  73.00   2.00    2.00    --   41.78 -77.00  30.00   13
  5  \w    -34.00  -8.00   2.00    2.00    --   41.78 -77.00  30.00   13
  6  \w     73.00 115.00   2.00    4.00    --  112.00-111.00  30.00   21
  7  \w     92.00 178.00   2.00    4.00    --  112.00  61.00 -30.00   43
  8  \w    110.00 166.00   2.00    4.00    --  112.00  30.00  60.00   28
  9  \w    106.00 178.00   2.00    4.00    --  112.00  30.00  30.00   36
 10  \w     41.00 115.00   2.00    4.00    --  112.00-111.00-150.00   37
 11  \w     83.00 109.00   2.00    4.00    --  112.00-111.00 120.00   13
 12  \w     41.00  69.00   2.00    4.00    --  112.00 -61.00 -90.00   14
 13  \w     78.00 140.00   2.00    4.00    --  112.00 -61.00 -90.00   31
 14  \w     83.00 131.00   2.00    4.00    --  112.00  61.00 -90.00   24
 15  \w     90.00 176.00   2.00    4.00    --  112.00  30.00 120.00   43
 16  \w     42.00 140.00   2.00    4.00    --  112.00 -61.00  30.00   49
 17  \w     36.00 134.00   2.00    4.00    --  112.00 -77.00-150.00   49
;
_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      -0.1384483000
_diffrn_orient_matrix_UB_12      -0.0266909000
_diffrn_orient_matrix_UB_13      -0.0623495000
_diffrn_orient_matrix_UB_21      0.0718105000
_diffrn_orient_matrix_UB_22      0.0958710000
_diffrn_orient_matrix_UB_23      -0.0289829000
_diffrn_orient_matrix_UB_31      0.0607149000
_diffrn_orient_matrix_UB_32      -0.0892576000
_diffrn_orient_matrix_UB_33      -0.0534480000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13092
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.975
_diffrn_reflns_theta_min         3.836
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.441
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.240
_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    1.612
_exptl_crystal_description       block
_exptl_crystal_F_000             1018
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.800
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         7471
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0749P)^2^+1.9810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7147
_reflns_number_total             7471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_no3_nd_no3_agno3_h2o_acet_red2
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        2060.2(3)
_cod_database_code               7232385
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C30 H32 O16 N6 Nd1'
_reflns_odcompleteness_completeness 99.51
_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. Restrained distances
 N48A-O49A \\sim N48A-O51A \\sim N48A-O50A
 with sigma of 0.02
 N48B-O51B \\sim N48B-O50B \\sim N48B-O49B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N48A) = Uanis(O50A) = Uanis(O49A) = Uanis(O51A)
Uanis(O49B) = Uanis(N48B) = Uanis(O51B) = Uanis(O50B)
4. Others
 Sof(N48B)=Sof(O51B)=Sof(O50B)=Sof(O49B)=Sof(O3WB)=1-FVAR(1)
 Sof(O3WA)=Sof(O3WC)=0.5*FVAR(2)
 Sof(N48A)=Sof(O49A)=Sof(O50A)=Sof(O51A)=FVAR(1)
 Sof(O42B)=Sof(O43B)=1-FVAR(2)
 Sof(O43A)=Sof(O42A)=FVAR(2)
 Sof(O47B)=1-FVAR(3)
 Sof(O47A)=FVAR(3)
5.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C20(H20A,H20B), C10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C35(H35), C36(H36), C16(H16), C23(H23), C13(H13),
 C12(H12), C15(H15), C22(H22), C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              2250
_shelx_fab_checksum              21841
_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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.818