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_7232370
_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 Sm, 1.39(Br), 1.61(C F3 O3 S)'
_chemical_formula_sum            'C31.61 H47 Br1.39 F4.84 N3 O20.84 S1.61 Sm'
_chemical_formula_weight         1207.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 102.696(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7334(4)
_cell_length_b                   25.6590(5)
_cell_length_c                   9.82867(19)
_cell_measurement_reflns_used    8435
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.1920
_cell_measurement_theta_min      4.1820
_cell_volume                     4608.93(16)
_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 0.996
_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   -114.00 -14.00   1.00   10.00    --  -41.65 -57.00-180.00  100
  2  \w    -22.00  83.00   1.00   10.00    --   41.65 -19.00   0.00  105
  3  \w     84.00 178.00   1.00   50.00    --  112.00  30.00 150.00   94
  4  \w     59.00 116.00   1.00   50.00    --  112.00-111.00   0.00   57
  5  \w     42.00 113.00   1.00   50.00    --  112.00-111.00-150.00   71
  6  \w     39.00 138.00   1.00   50.00    --  112.00 -45.00 -30.00   99
  7  \w     43.00 100.00   1.00   50.00    --  112.00-111.00 -60.00   57
  8  \w    101.00 164.00   1.00   50.00    --  112.00 111.00 -30.00   63
;
_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      0.0786849000
_diffrn_orient_matrix_UB_12      0.0139017000
_diffrn_orient_matrix_UB_13      0.0756247000
_diffrn_orient_matrix_UB_21      -0.0301103000
_diffrn_orient_matrix_UB_22      0.0396544000
_diffrn_orient_matrix_UB_23      0.0909920000
_diffrn_orient_matrix_UB_31      -0.0022059000
_diffrn_orient_matrix_UB_32      -0.0429681000
_diffrn_orient_matrix_UB_33      0.1085102000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16613
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.996
_diffrn_reflns_theta_min         2.969
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.543
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.285
_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    1.740
_exptl_crystal_description       plate
_exptl_crystal_F_000             2417
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.974
_refine_diff_density_min         -1.831
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         8360
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0801P)^2^+17.8554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7190
_reflns_number_total             8360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01015c2.cif
_cod_data_source_block           jj003_br_sm_otf_kotfx6_h2o_acet_mp_red2
_cod_depositor_comments
'Adding full bibliography for 7232365--7232385.cif.'
_cod_original_cell_volume        4608.92(16)
_cod_database_code               7232370
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C32 H31 Br2 F5 N3 Sm1 O13 S1'
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.188
_reflns_odcompleteness_completeness 99.36
_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. Uiso/Uaniso restraints and constraints
Uanis(O43) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O42) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Br2B)=1-FVAR(1)
 Sof(S48A)=Sof(F54A)=Sof(O50A)=Sof(O49A)=Sof(F53A)=Sof(F55A)=Sof(O51A)=
 Sof(C52A)=FVAR(1)
4.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C20(H20A,H20B), C10(H10A,H10B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C13(H13), C35(H35), C12(H12), C32(H32), C36(H36), C25(H25),
 C16(H16), C22(H22), C26(H26), C33(H33), C23(H23)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              93493
_shelx_fab_checksum              10168
_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 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.703