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_7232377
_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(Br)'
_chemical_formula_sum            'C30 H45 Br3 N3 Nd O15'
_chemical_formula_weight         1071.66
_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             2018-03-28
_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                104.683(2)
_cell_angle_beta                 98.809(2)
_cell_angle_gamma                99.428(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4378(3)
_cell_length_b                   12.3546(3)
_cell_length_c                   18.8810(4)
_cell_measurement_reflns_used    8623
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.0950
_cell_measurement_theta_min      3.8560
_cell_volume                     2056.69(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 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    -66.00  27.00   1.00    1.00    --  -41.65  57.00  60.00   93
  2  \w      1.00  82.00   1.00    1.00    --   41.65 -99.00 150.00   81
  3  \w     36.00  63.00   1.00    1.50    --  112.00-111.00  30.00   27
  4  \w     83.00 115.00   1.00    1.50    --  112.00-111.00  30.00   32
  5  \w     66.00 105.00   1.00    1.50    --  112.00 -94.00 -60.00   39
  6  \w     57.00 141.00   1.00    1.50    --  112.00 -61.00 -30.00   84
  7  \w     65.00 171.00   1.00    1.50    --  112.00  15.00  60.00  106
  8  \w    149.00 178.00   1.00    1.50    --  112.00  61.00 -30.00   29
  9  \w    110.00 177.00   1.00    1.50    --  112.00  61.00 -60.00   67
 10  \w     87.00 168.00   1.00    1.50    --  112.00  45.00 -90.00   81
 11  \w     83.00 115.00   1.00    1.50    --  112.00  61.00 -30.00   32
 12  \w     45.00 135.00   1.00    1.50    --  112.00 -61.00-180.00   90
 13  \w     50.00 116.00   1.00    1.50    --  112.00-111.00-150.00   66
 14  \w     42.00 102.00   1.00    1.50    --  112.00-111.00 150.00   60
 15  \w   -115.00 -17.00   1.00    1.00    --  -41.65 -37.00 150.00   98
 16  \w   -113.00 -20.00   1.00    1.00    --  -41.65 -57.00 -90.00   93
;
_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      0.1608776000
_diffrn_orient_matrix_UB_12      0.0355007000
_diffrn_orient_matrix_UB_13      -0.0061775000
_diffrn_orient_matrix_UB_21      0.0269374000
_diffrn_orient_matrix_UB_22      -0.1171922000
_diffrn_orient_matrix_UB_23      0.0062767000
_diffrn_orient_matrix_UB_31      -0.0442825000
_diffrn_orient_matrix_UB_32      -0.0490283000
_diffrn_orient_matrix_UB_33      -0.0857078000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12580
_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         67.992
_diffrn_reflns_theta_min         3.785
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.614
_exptl_absorpt_correction_T_max  0.422
_exptl_absorpt_correction_T_min  0.117
_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    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             1062
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.073
_refine_diff_density_max         1.727
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         7446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0652P)^2^+6.7132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7176
_reflns_number_total             7446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_nd_br_h2o_acet_red3
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        2056.71(10)
_cod_database_code               7232377
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C21 H25 O8 Nd Br3 N3'
_reflns_odcompleteness_completeness 99.44
_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(Br3A)=FVAR(1)
3.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C30(H30A,H30B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C15(H15), C35(H35), C32(H32), C33(H33), C23(H23),
 C13(H13), C36(H36), C22(H22), C26(H26), C25(H25)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              4000
_shelx_fab_checksum              91602
_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 1.369
_oxdiff_exptl_absorpt_empirical_full_min 0.778