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_7232367
_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         'C60 H59 N6 O10, 5(Br), 4(H2 O), 2(O)'
_chemical_formula_sum            'C60 H67 Br5 N6 O16'
_chemical_formula_weight         1527.74
_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             2018-03-06
_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                103.662(4)
_cell_angle_beta                 114.054(5)
_cell_angle_gamma                106.336(4)
_cell_formula_units_Z            1
_cell_length_a                   11.1828(6)
_cell_length_b                   13.1617(5)
_cell_length_c                   13.3823(7)
_cell_measurement_reflns_used    5073
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      28.6490
_cell_measurement_theta_min      1.7620
_cell_volume                     1581.64(18)
_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      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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    -57.00  35.00   1.00   15.00    --    8.98 -57.00 -90.00   92
  2  \w    -16.00  81.00   1.00   15.00    --    8.98  57.00  60.00   97
  3  \w    -20.00  50.00   1.00   15.00    --    8.98 -99.00-180.00   70
;
_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      0.0101359000
_diffrn_orient_matrix_UB_12      -0.0474036000
_diffrn_orient_matrix_UB_13      -0.0275326000
_diffrn_orient_matrix_UB_21      -0.0430462000
_diffrn_orient_matrix_UB_22      -0.0010724000
_diffrn_orient_matrix_UB_23      -0.0568388000
_diffrn_orient_matrix_UB_31      0.0627336000
_diffrn_orient_matrix_UB_32      0.0388273000
_diffrn_orient_matrix_UB_33      0.0048443000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11112
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.997
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.759
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.248
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.559
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       plank
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6149
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0313P)^2^+3.0141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5077
_reflns_number_total             6149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_br_nd_otf_koh_h2o_test1_red3
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        1581.63(14)
_cod_database_code               7232367
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.364
_reflns_odcompleteness_completeness 97.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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) groups, All O(H,H) groups
2. Restrained distances
 O39A-H38A_$1
 1.4 with sigma of 0.02
 O38A-H38A
 1.3 with sigma of 0.02
 C37-O39C
 1.2 with sigma of 0.02
3. Restrained planarity
 O39C, C37, O38C, C34
 with sigma of 0.1
 O39B, O38B, C37, C34
 with sigma of 0.1
 O38C, C37, O39C, C34
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(O38B) \\sim Ueq, Uanis(O38A) \\sim Ueq, Uanis(O38C) \\sim Ueq,
Uanis(O39B) \\sim Ueq, Uanis(O39A) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(O39C)
\\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(O38B) = Uanis(O38A) = Uanis(O38C)
Uanis(O39B) = Uanis(O39A) = Uanis(O39C)
5. Others
 Fixed Sof: O38A(0.5) H38A(0.5) O39A(0.5) O38B(0.3) O39B(0.3) O38C(0.2)
 O39C(0.2)
 Fixed Uiso: H38A(0.05)
6.a Free rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C30(H30A,H30B)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C35(H35), C36(H36)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
6.e Idealised tetrahedral OH refined as rotating group:
 O19(H19), O29(H29)
;
_shelx_res_checksum              25038
_olex2_exptl_crystal_mounting_method 'Mitegen loop 100 micron'
_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 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.753