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_7232382
_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 H62 N6 O17 Sm2, 0.1(Br), 5.9(C F3 O3 S), 0.75(O)'
_chemical_formula_sum            'C65.9 H86 Br0.1 F17.7 N6 O47.45 S5.9 Sm2'
_chemical_formula_weight         2555.55
_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                89.1178(19)
_cell_angle_beta                 87.111(2)
_cell_angle_gamma                87.308(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1269(3)
_cell_length_b                   14.2176(4)
_cell_length_c                   34.2981(6)
_cell_measurement_reflns_used    9569
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      76.5740
_cell_measurement_theta_min      2.5520
_cell_volume                     4926.1(2)
_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      123.00(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 0.992
_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   -118.00  -9.00   1.00    8.00    --  -41.78 -77.00  90.00  109
  2  \w   -116.00 -17.00   1.00    8.00    --  -41.78 -37.00 -30.00   99
  3  \w      1.00  83.00   1.00    8.00    --   41.78 -99.00 -60.00   82
  4  \w      1.00  62.00   1.00    8.00    --   41.78 -99.00-150.00   61
  5  \w     36.00 145.00   1.00   50.00    --  112.00 -77.00 -30.00  109
  6  \w     41.00 116.00   1.00   50.00    --  112.00-111.00 150.00   75
  7  \w     38.00  77.00   1.00   50.00    --  112.00 -30.00 -60.00   39
  8  \w     31.00 165.00   1.00   50.00    --  112.00 -15.00  90.00  134
  9  \w     31.00 109.00   1.00   50.00    --  112.00 -94.00 -90.00   78
 10  \w     45.00  91.00   1.00   50.00    --  112.00 -30.00 -30.00   46
 11  \w    106.00 169.00   1.00   50.00    --  112.00 111.00  60.00   63
 12  \w     41.00 126.00   1.00   50.00    --  112.00 -61.00 120.00   85
 13  \w     86.00 174.00   1.00   50.00    --  112.00  45.00 120.00   88
;
_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      -0.0979786000
_diffrn_orient_matrix_UB_12      0.0860599000
_diffrn_orient_matrix_UB_13      0.0033042000
_diffrn_orient_matrix_UB_21      0.1098259000
_diffrn_orient_matrix_UB_22      0.0642542000
_diffrn_orient_matrix_UB_23      -0.0154456000
_diffrn_orient_matrix_UB_31      -0.0398664000
_diffrn_orient_matrix_UB_32      -0.0153006000
_diffrn_orient_matrix_UB_33      -0.0421132000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0940
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            29760
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         3.112
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.237
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_correction_T_min  0.410
_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    1.723
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.639
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1256
_refine_ls_number_reflns         17807
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+8.1554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14021
_reflns_number_total             17807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003-01-sm-otf-h2o-red6
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_formula_sum
'C65.90 H86 Br0.10 F17.70 N6 O47.45 S5.90 Sm2'
_cod_database_code               7232382
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C21 H20 O9 N3 F3 Sm S2'
_reflns_odcompleteness_completeness 99.35
_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. Shared sites
{O38A, O39B}
3. Restrained distances
 C34B-C37B
 1.53 with sigma of 0.02
 C37B-O38B
 1.25 with sigma of 0.02
 C37B-O39B
 1.25 with sigma of 0.02
 H4WA-O11A
 1.7 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O38A) = Uanis(O39B)
Uanis(C35B) = Uanis(C36B) = Uanis(N31B) = Uanis(C32B) = Uanis(C33B) =
Uanis(C34B) = Uanis(C37B) = Uanis(O38B)
Uanis(O12B) = Uanis(O10A)
Uanis(F16B) = Uanis(C13B) = Uanis(F14B) = Uanis(F15B)
Uanis(F16A) = Uanis(C13A) = Uanis(F15A) = Uanis(F14A)
Uanis(C5A) = Uanis(F7A) = Uanis(F7B) = Uanis(F6A)
Uanis(C5B) = Uanis(F6B) = Uanis(F7B) = Uanis(F8B)
Uanis(O3B) = Uanis(O2B) = Uanis(O4B)
Uanis(C32A) = Uanis(C33A) = Uanis(C36A) = Uanis(C35A) = Uanis(C35B) =
Uanis(N31A) = Uanis(C37A) = Uanis(O39B) = Uanis(O39A)
Uanis(O6WA) = Uanis(O6WB)
5. Others
 Sof(C5B)=Sof(F8B)=Sof(F6B)=Sof(F7B)=Sof(O4B)=Sof(O3B)=Sof(O2B)=Sof(S1B)=1-
 FVAR(1)
 Sof(C5A)=Sof(F7A)=Sof(F8A)=Sof(F6A)=Sof(O4A)=Sof(O2A)=Sof(O3A)=Sof(S1A)=FVAR(1)
 Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=Sof(N31B)=Sof(C32B)=Sof(H32B)=
 Sof(C33B)=Sof(H33B)=Sof(C34B)=Sof(C37B)=Sof(O38B)=Sof(O39B)=1-FVAR(2)
 Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36A)=Sof(C37A)=Sof(N31A)=Sof(O38A)=Sof(O39A)=FVAR(2)
 Fixed Sof: Br1C(0.1) C13A(0.65) F14A(0.65) F16A(0.65) F15A(0.65) O10A(0.65)
 O12A(0.65) O11A(0.65) S9A(0.65) C13B(0.25) F14B(0.25) F16B(0.25) F15B(0.25)
 O12B(0.25) O10B(0.25) O11B(0.25) S9B(0.25) O6WB(0.375) O6WA(0.375)
6.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
6.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C20(H20A,H20B), C49(H49A,H49B), C59(H59A,H59B), C69(H69A,H69B)
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), C32A(H32A), C33A(H33A), C35A(H35A), C35B(H35B), C36B(H36B),
 C32B(H32B), C33B(H33B), C36A(H36A), C51(H51), C52(H52), C54(H54), C55(H55),
 C61(H61), C62(H62), C64(H64), C65(H65), C71(H71), C72(H72), C74(H74), C75(H75)
6.d Fitted hexagon refined as free rotating group:
 C35B(C36B,N31B,C32B,C33B,C34B)
6.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              54292
_shelx_fab_checksum              3271
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.384
_oxdiff_exptl_absorpt_empirical_full_min 0.718