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_7232369
_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 Gd N3 O8, 2(Br), C F3 O3 S'
_chemical_formula_sum            'C31 H51 Br2 F3 Gd N3 O21 S'
_chemical_formula_weight         1207.88
_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             2018-03-26
_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                107.797(4)
_cell_angle_beta                 103.227(4)
_cell_angle_gamma                99.461(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5280(4)
_cell_length_b                   14.3123(6)
_cell_length_c                   18.8610(8)
_cell_measurement_reflns_used    7885
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.6790
_cell_measurement_theta_min      3.3350
_cell_volume                     2306.55(19)
_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 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -70.00  31.00   1.00    1.00    --  -41.90  57.00 -30.00  101
  2  \w    -74.00  33.00   1.00    1.00    --  -41.90  77.00-180.00  107
  3  \w     52.00 103.00   1.00    1.00    --   41.90-138.00 117.00   51
  4  \w     61.00 141.00   1.00    2.00    --  112.00 -61.00 150.00   80
  5  \w     64.00 108.00   1.00    2.00    --  112.00 -94.00  60.00   44
  6  \w     51.00 136.00   1.00    2.00    --  112.00 -45.00  60.00   85
  7  \w     75.00 108.00   1.00    2.00    --  112.00 -94.00-120.00   33
  8  \w     65.00 115.00   1.00    2.00    --  112.00-111.00-180.00   50
  9  \w     41.00 132.00   1.00    2.00    --  112.00 -45.00 -30.00   91
 10  \w     29.00  55.00   1.00    2.00    --  112.00 -94.00-120.00   26
 11  \w     29.00 109.00   1.00    2.00    --  112.00 -94.00 -30.00   80
 12  \w     30.00 178.00   1.00    2.00    --  112.00   0.00 120.00  148
 13  \w    100.00 172.00   1.00    2.00    --  112.00 111.00 120.00   72
 14  \w   -113.00 -18.00   1.00    1.00    --  -41.90 -37.00  30.00   95
;
_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      -0.1048011000
_diffrn_orient_matrix_UB_12      -0.0828012000
_diffrn_orient_matrix_UB_13      -0.0759865000
_diffrn_orient_matrix_UB_21      -0.0649963000
_diffrn_orient_matrix_UB_22      -0.0558804000
_diffrn_orient_matrix_UB_23      0.0478813000
_diffrn_orient_matrix_UB_31      -0.1194279000
_diffrn_orient_matrix_UB_32      0.0606128000
_diffrn_orient_matrix_UB_33      0.0022511000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14103
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         2.577
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.555
_exptl_absorpt_correction_T_max  0.269
_exptl_absorpt_correction_T_min  0.061
_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    1.739
_exptl_crystal_description       block
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.132
_refine_diff_density_max         2.858
_refine_diff_density_min         -1.928
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1298P)^2^+11.1175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.1984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7753
_reflns_number_total             8343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_br_gd_otf_h2o_acet_red3
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        2306.53(18)
_cod_database_code               7232369
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C21 H25 O12 N3 F12 S3 Br1 Gd1'
_chemical_oxdiff_usercomment     'clear colorless block'
_reflns_odcompleteness_completeness 99.32
_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(Br2B)=1-FVAR(1)
 Sof(Br2A)=FVAR(1)
3.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C10(H10A,H10B), C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C23(H23), C32(H32), C25(H25), C22(H22), C15(H15), C12(H12),
 C13(H13), C33(H33), C36(H36), C26(H26), C35(H35)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              51924
_shelx_fab_checksum              99322
_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 1.708
_oxdiff_exptl_absorpt_empirical_full_min 0.600