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_7232376
_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 O8 Yb, 2.9(C F3 O3 S), 0.1(Br)'
_chemical_formula_sum            'C32.9 H41 Br0.1 F8.7 N3 O21.7 S2.9 Yb'
_chemical_formula_weight         1264.99
_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                109.018(3)
_cell_angle_beta                 105.086(3)
_cell_angle_gamma                95.287(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0256(3)
_cell_length_b                   14.2571(4)
_cell_length_c                   18.5311(5)
_cell_measurement_reflns_used    10585
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.3350
_cell_measurement_theta_min      4.5710
_cell_volume                     2372.01(14)
_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 0.993
_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   -116.00 -17.00   1.00    2.50    --  -41.78 -37.00-180.00   99
  2  \w   -116.00 -23.00   1.00    2.50    --  -41.78 -37.00  90.00   93
  3  \w      1.00  49.00   1.00    2.50    --   41.78 -99.00  60.00   48
  4  \w      1.00  62.00   1.00    2.50    --   41.78 -99.00 -30.00   61
  5  \w     53.00  97.00   1.00    2.50    --   41.78-125.00-180.00   44
  6  \w     66.00 109.00   1.00    7.50    --  112.00 -94.00-120.00   43
  7  \w     50.00 109.00   1.00    7.50    --  112.00 -94.00 -60.00   59
  8  \w     65.00 150.00   1.00    7.50    --  112.00 178.00-180.00   85
  9  \w    148.00 176.00   1.00    7.50    --  112.00 111.00 120.00   28
 10  \w     73.00 149.00   1.00    7.50    --  112.00 178.00 150.00   76
 11  \w     83.00 166.00   1.00    7.50    --  112.00  61.00 -90.00   83
 12  \w     32.00 151.00   1.00    7.50    --  112.00 -15.00  90.00  119
 13  \w     40.00 116.00   1.00    7.50    --  112.00-111.00 150.00   76
 14  \w     44.00 136.00   1.00    7.50    --  112.00 -61.00 120.00   92
 15  \w     36.00 140.00   1.00    7.50    --  112.00 -30.00-120.00  104
;
_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      0.1025755000
_diffrn_orient_matrix_UB_12      0.0063778000
_diffrn_orient_matrix_UB_13      -0.0481056000
_diffrn_orient_matrix_UB_21      0.1187461000
_diffrn_orient_matrix_UB_22      -0.0146606000
_diffrn_orient_matrix_UB_23      0.0649433000
_diffrn_orient_matrix_UB_31      -0.0411655000
_diffrn_orient_matrix_UB_32      -0.1154024000
_diffrn_orient_matrix_UB_33      -0.0448677000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14829
_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         67.995
_diffrn_reflns_theta_min         3.428
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.989
_exptl_absorpt_correction_T_max  0.828
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.771
_exptl_crystal_description       prism
_exptl_crystal_F_000             1262
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.995
_refine_diff_density_min         -7.199
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         8573
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0822
_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^)+(0.1894P)^2^+10.0617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7681
_reflns_number_total             8573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_br_yb_otf_kotfx6_h2o_acet_red3_clark
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        2372.01(13)
_cod_original_formula_sum        'C32.90 H41 Br0.10 F8.70 N3 O21.70 S2.90 Yb'
_cod_database_code               7232376
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C33 H34 F9 N3 O17 S3 Yb1'
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.503
_reflns_odcompleteness_completeness 99.16
_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
 H2WB-O59A
 2 with sigma of 0.02
 O58A_$1-H1WB
 1.95 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F53A) \\sim Ueq, Uanis(O50A) \\sim Ueq, Uanis(S48A) \\sim Ueq,
Uanis(C52A) \\sim Ueq, Uanis(O49A) \\sim Ueq, Uanis(O51A) \\sim Ueq,
Uanis(F55A) \\sim Ueq, Uanis(F54A) \\sim Ueq, Uanis(F53B) \\sim Ueq,
Uanis(S48B) \\sim Ueq, Uanis(O49B) \\sim Ueq, Uanis(O51B) \\sim Ueq,
Uanis(C52B) \\sim Ueq, Uanis(O50B) \\sim Ueq, Uanis(F54B) \\sim Ueq,
Uanis(F55B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O19) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(C27)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 F53B, S48B, O49B, O51B, C52B, O50B, F54B, F55B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F53A, O50A, S48A, C52A, O49A, O51A, F55A, F54A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S48B)=Sof(O49B)=Sof(F54B)=Sof(O51B)=Sof(F55B)=Sof(C52B)=Sof(F53B)=
 Sof(O50B)=1-FVAR(1)
 Sof(O50A)=Sof(F53A)=Sof(C52A)=Sof(F55A)=Sof(S48A)=Sof(O49A)=Sof(O51A)=
 Sof(F54A)=FVAR(1)
 Fixed Sof: S56A(0.9) O58A(0.9) O59A(0.9) F61A(0.9) F63A(0.9) O57A(0.9)
 F62A(0.9) C60A(0.9) Br1B(0.1)
6.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
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:
 C25(H25), C12(H12), C26(H26), C13(H13), C32(H32), C33(H33), C35(H35),
 C22(H22), C23(H23), C36(H36), C16(H16), C15(H15)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              62937
_shelx_fab_checksum              3616
_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 2.800
_oxdiff_exptl_absorpt_empirical_full_min 0.628