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_7713155
_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         'C96 H151 O36 P6 Pr2, I3, 2(C2 H6 O)'
_chemical_formula_sum            'C100 H163 I3 O38 P6 Pr2'
_chemical_formula_weight         2821.63
_chemical_name_systematic        'Pr Crown'
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2fsj3w
_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                111.8356(12)
_cell_angle_beta                 90.6420(10)
_cell_angle_gamma                111.7694(12)
_cell_formula_units_Z            1
_cell_length_a                   14.33192(19)
_cell_length_b                   15.0410(2)
_cell_length_c                   17.6013(2)
_cell_measurement_reflns_used    69204
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.6950
_cell_measurement_theta_min      2.2880
_cell_volume                     3221.53(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -84.00  58.00   1.00   10.00    --    5.00 -21.00 -31.00  142
  2  \w    -68.00  75.00   1.00   10.00    --  -14.30  21.00 134.00  143
  3  \w   -104.00  24.00   1.00   10.00    --  -14.30 -72.00 -30.00  128
  4  \w    -48.00  75.00   1.00   10.00    --  -14.30  38.00 150.00  123
  5  \w   -104.00  21.00   1.00   10.00    --  -14.30 -57.00-150.00  125
  6  \w    -48.00  75.00   1.00   10.00    --  -14.30  38.00  90.00  123
  7  \w   -104.00  24.00   1.00   10.00    --  -14.30 -72.00-180.00  128
  8  \w    -53.00  75.00   1.00   10.00    --  -14.30  72.00   0.00  128
  9  \w   -104.00  21.00   1.00   10.00    --  -14.30 -57.00  30.00  125
 10  \w    -53.00  75.00   1.00   10.00    --  -14.30  72.00 150.00  128
 11  \w    -53.00  75.00   1.00   10.00    --  -14.30  72.00  30.00  128
 12  \w    -53.00  75.00   1.00   10.00    --  -14.30  72.00 -90.00  128
 13  \w    -53.00  50.00   1.00   10.00    --  -14.30  72.00-150.00  103
 14  \w    -50.00  75.00   1.00   10.00    --  -14.30  57.00 -90.00  125
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0455194000
_diffrn_orient_matrix_UB_12      0.0325649000
_diffrn_orient_matrix_UB_13      -0.0081217000
_diffrn_orient_matrix_UB_21      -0.0263892000
_diffrn_orient_matrix_UB_22      0.0272704000
_diffrn_orient_matrix_UB_23      -0.0094273000
_diffrn_orient_matrix_UB_31      0.0126179000
_diffrn_orient_matrix_UB_32      0.0357818000
_diffrn_orient_matrix_UB_33      0.0422846000
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            121284
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.404
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
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    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1434
_exptl_crystal_preparation       'In the manuscript'
_exptl_crystal_recrystallization_method 'In the manuscript'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.845
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         11252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+6.6962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10770
_reflns_number_total             11252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01206a2.cif
_cod_data_source_block           adi-410-pr-crown-dipp-re
_cod_original_cell_volume        3221.52(8)
_cod_database_code               7713155
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pr C O P I '
_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: H12(0.5) I2A(0.65) I2B(0.35)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C31(H31), C34(H34)
3.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
 C50(H50A,H50B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16A), C17(H17), C27(H27), C28(H28),
 C29(H29), C40(H40), C41(H41), C42(H42)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C49(H49A,H49B,H49C)
3.e Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12), O16(H16), O19(H19A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 104 electrons were 
found in a volume of 266\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CH3CH2OH] per Asymmetric Unit 
which account for 104 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              12055
_shelx_fab_checksum              40357
_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 2.145
_oxdiff_exptl_absorpt_empirical_full_min 0.534