Field-Induced SIM Behaviour in Early Lanthanide(III) Organophosphates Incorporating 18-crown-6
Borah, Aditya; Dey, Sourav; Gupta, Sandeep Kumar; Rajaraman, Gopalan; Murugavel, Ramaswamy; Dalton Transactions  (2023) –; doi:10.1039/D3DT01206A

data_7713156
_publ_section_title
;
 Field-Induced SIM Behaviour in Early Lanthanide(III) Organophosphates
 Incorporating 18-crown-6
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01206A
_journal_year                    2023
_chemical_formula_moiety         '2(C48 H78.5 Nd O18 P3), I3, C H3 O'
_chemical_formula_sum            'C97 H160 I3 Nd2 O37 P6'
_chemical_formula_weight         2773.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2fsj4x
_audit_creation_date             2023-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-20 deposited with the CCDC.	2023-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                67.693(5)
_cell_angle_beta                 88.567(4)
_cell_angle_gamma                63.094(6)
_cell_formula_units_Z            1
_cell_length_a                   14.3480(8)
_cell_length_b                   15.8035(9)
_cell_length_c                   17.2262(8)
_cell_measurement_reflns_used    20275
_cell_measurement_temperature    123(30)
_cell_measurement_theta_max      28.4760
_cell_measurement_theta_min      1.7100
_cell_volume                     3171.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123(30)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -349.73  10.27   0.80    3.00   9.41 -12.98 -31.50    --   450
  2  \w    -68.96  -0.16   0.80    3.00    --  -19.47  94.56 -34.84   86
  3  \w    -65.46   0.14   0.80    3.00    --  -15.96  94.56 145.16   82
  4  \w   -108.63  15.37   0.80    3.00    --  -12.98 -59.25 173.08  155
  5  \f    -10.27 349.73   0.80    3.00  77.88 -12.98  31.50    --   450
  6  \w    -65.46   0.14   0.80    3.00    --  -15.96  94.56  73.16   82
  7  \w    -55.98   0.02   0.80    3.00    --   -6.49  94.56 -34.84   70
  8  \w   -108.63  15.37   0.80    3.00    --  -12.98 -59.25 -33.92  155
  9  \f   -339.92  20.08   0.80    3.00  16.12 -12.98 -59.25    --   450
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0027436000
_diffrn_orient_matrix_UB_12      0.0386402000
_diffrn_orient_matrix_UB_13      0.0097883000
_diffrn_orient_matrix_UB_21      -0.0372355000
_diffrn_orient_matrix_UB_22      0.0393946000
_diffrn_orient_matrix_UB_23      -0.0376261000
_diffrn_orient_matrix_UB_31      -0.0421860000
_diffrn_orient_matrix_UB_32      0.0030940000
_diffrn_orient_matrix_UB_33      0.0231044000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            121941
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.247
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.25616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             1407
_exptl_crystal_preparation       0
_exptl_crystal_recrystallization_method .00
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.998
_refine_diff_density_min         -2.271
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         11155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0969P)^2^+16.0345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8722
_reflns_number_total             11155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01206a2.cif
_cod_data_source_block           adi_5_618_nd_c_d_autored
_cod_original_cell_volume        3171.1(3)
_cod_database_code               7713156
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.729
_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
2. Others
 Fixed Sof: H7(0.5) I1(0.1) I1A(0.1) I1B(0.8) O19(0.5) C50(0.5) H50B(0.5)
 H50C(0.5) H50A(0.5)
3.a Ternary CH refined with riding coordinates:
 C7(H7A), C11(H11A), C32(H32), C35(H35), C44(H44), C47(H47)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C5(H5), C28(H28), C29(H29), C30(H30), C40(H40), C41(H41),
 C42(H42)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C50(H50B,H50C,H50A)
3.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O6(H6), O7(H7), O11(H11)
;
_smtbx_masks_special_details
;
3[CH3OH] 
2 [H2O]
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61101
_shelx_fab_checksum              78064
_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 2.475
_oxdiff_exptl_absorpt_empirical_full_min 0.547