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_7232379
_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
'C30.57 H28.7 F1.72 N3 Nd O8.57 S0.57, 2(Br), 0.43(C1 F3 O3 S1), 1.15(H2 O)'
_chemical_formula_sum            'C31 H31 Br2 F3 N3 Nd O11 S'
_chemical_formula_weight         1014.71
_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             2018-05-09
_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                105.103(2)
_cell_angle_beta                 98.057(2)
_cell_angle_gamma                99.489(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4141(3)
_cell_length_b                   12.0776(3)
_cell_length_c                   18.7454(5)
_cell_measurement_reflns_used    8785
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.1580
_cell_measurement_theta_min      3.8660
_cell_volume                     1991.70(10)
_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 5.1977
_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   -116.00 -17.00   1.00    2.00    --  -41.65 -37.00  90.00   99
  2  \w   -114.00 -15.00   1.00    2.00    --  -41.65 -57.00-150.00   99
  3  \w    -62.00  23.00   1.00    2.00    --  -41.65  57.00   0.00   85
  4  \w      1.00  83.00   1.00    2.00    --   41.65 -99.00  90.00   82
  5  \w     41.00 141.00   1.00    8.00    --  112.00 -61.00-150.00  100
  6  \w     58.00 116.00   1.00    8.00    --  112.00-111.00 150.00   58
  7  \w     35.00  61.00   1.00    8.00    --  112.00 -94.00 -30.00   26
  8  \w     39.00  90.00   1.00    8.00    --  112.00 -45.00 150.00   51
  9  \w     43.00 129.00   1.00    8.00    --  112.00 -45.00   0.00   86
 10  \w     30.00 106.00   1.00    8.00    --  112.00 -94.00  30.00   76
 11  \w     91.00 176.00   1.00    8.00    --  112.00  30.00 -60.00   85
 12  \w     70.00 101.00   1.00    8.00    --  112.00 -94.00 -30.00   31
 13  \w     30.00  96.00   1.00    8.00    --  112.00 -94.00-180.00   66
 14  \w    114.00 141.00   1.00    8.00    --  112.00 111.00 -60.00   27
 15  \w     77.00 114.00   1.00    8.00    --  112.00-111.00 -90.00   37
 16  \w     60.00 178.00   1.00    8.00    --  112.00  15.00  60.00  118
;
_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      0.1497051000
_diffrn_orient_matrix_UB_12      0.0250949000
_diffrn_orient_matrix_UB_13      -0.0234399000
_diffrn_orient_matrix_UB_21      -0.0751209000
_diffrn_orient_matrix_UB_22      0.0258400000
_diffrn_orient_matrix_UB_23      -0.0705738000
_diffrn_orient_matrix_UB_31      0.0230132000
_diffrn_orient_matrix_UB_32      0.1302635000
_diffrn_orient_matrix_UB_33      0.0446568000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0382
_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       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12783
_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         67.989
_diffrn_reflns_theta_min         3.878
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.409
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.456
_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    1.692
_exptl_crystal_description       prism
_exptl_crystal_F_000             998
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7241
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0477P)^2^+3.4615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7009
_reflns_number_total             7241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_br_nd_otf_h2o_acet_evac_ii_red2
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        1991.69(9)
_cod_database_code               7232379
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C33 H30 N3 O12 S1 F3 Nd1'
_shelx_estimated_absorpt_t_max   0.637
_shelx_estimated_absorpt_t_min   0.259
_reflns_odcompleteness_completeness 99.56
_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. Shared sites
{O1WB, O51A}
{O2WB, O50A}
3. Restrained distances
 H4WA-Br2B
 2.55 with sigma of 0.04
 H4WB-Br1B
 2.55 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(O41A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1WB) = Uanis(O51A)
Uanis(O2WB) = Uanis(O50A)
5. Others
 Sof(S40A)=Sof(F45A)=Sof(F47A)=Sof(F46A)=Sof(C44A)=Sof(Br1B)=Sof(O42A)=
 Sof(O41A)=Sof(H1WA)=Sof(H1WB)=Sof(O2WB)=Sof(H2WA)=Sof(H2WB)=Sof(O43A)=
 Sof(O1WB)=1-FVAR(1)
 Sof(Br2B)=Sof(S48A)=Sof(O49A)=Sof(F54A)=Sof(F53A)=Sof(F55A)=Sof(C52A)=
 Sof(O3WA)=Sof(H3WA)=Sof(H3WB)=Sof(O51A)=Sof(O4WB)=Sof(H4WA)=Sof(H4WB)=
 Sof(O50A)=FVAR(1)
6.a Free rotating group:
 O3WA(H3WA,H3WB), O4WB(H4WA,H4WB)
6.b Rotating group:
 O51A(H1WA,H1WB), O2WB(H2WA,H2WB)
6.c Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C30(H30A,H30B), C10(H10A,H10B)
6.d Aromatic/amide H refined with riding coordinates:
 C26(H26), C35(H35), C32(H32), C33(H33), C22(H22), C25(H25), C23(H23),
 C36(H36), C13(H13), C16(H16), C12(H12), C15(H15)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              82698
_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 3.216
_oxdiff_exptl_absorpt_empirical_full_min 0.806