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_7713153
_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 H155 Ce2 O36 P6, I3, 2(C O)'
_chemical_formula_sum            'C98 H155 Ce2 I3 O38 P6'
_chemical_formula_weight         2787.97
_chemical_name_systematic        Ce_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2fsj2v
_audit_creation_date             2023-04-04
_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                108.616(2)
_cell_angle_beta                 98.084(2)
_cell_angle_gamma                106.682(2)
_cell_formula_units_Z            1
_cell_length_a                   14.6386(3)
_cell_length_b                   15.8305(5)
_cell_length_c                   16.1766(4)
_cell_measurement_reflns_used    15862
_cell_measurement_temperature    150
_cell_measurement_theta_max      21.2240
_cell_measurement_theta_min      2.2870
_cell_volume                     3289.79(17)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_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  \w    -84.00  40.00   1.00   10.00    --    5.00 -54.00 109.00  124
  2  \w    -50.00  75.00   1.00   10.00    --  -14.30  54.00-106.00  125
  3  \w   -104.00  24.00   1.00   10.00    --  -14.30 -72.00 -30.00  128
  4  \w   -104.00  21.00   1.00   10.00    --  -14.30 -57.00-180.00  125
  5  \w   -104.00  24.00   1.00   10.00    --  -14.30 -72.00  30.00  128
  6  \w    -48.00  75.00   1.00   10.00    --  -14.30  38.00 -60.00  123
  7  \w   -104.00  21.00   1.00   10.00    --  -14.30 -54.00 109.00  125
  8  \w    -50.00  75.00   1.00   10.00    --  -14.30  57.00-180.00  125
  9  \w    -53.00  75.00   1.00   10.00    --  -14.30  72.00 -30.00  128
 10  \w    -53.00  75.00   1.00   10.00    --  -14.30  72.00  90.00  128
 11  \w    -53.00 -19.00   1.00   10.00    --  -14.30  72.00-150.00   34
 12  \w    -53.00  75.00   1.00   10.00    --  -14.30  72.00  60.00  128
;
_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      -0.0289404000
_diffrn_orient_matrix_UB_12      -0.0044556000
_diffrn_orient_matrix_UB_13      0.0311058000
_diffrn_orient_matrix_UB_21      0.0115868000
_diffrn_orient_matrix_UB_22      -0.0402234000
_diffrn_orient_matrix_UB_23      0.0011267000
_diffrn_orient_matrix_UB_31      0.0420248000
_diffrn_orient_matrix_UB_32      0.0302892000
_diffrn_orient_matrix_UB_33      0.0363571000
_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  0.0954
_diffrn_reflns_av_unetI/netI     0.0556
_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       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            100090
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.273
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53906
_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            'reddish brown'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             1412
_exptl_crystal_preparation       'in the manuscript'
_exptl_crystal_recrystallization_method 'in the manuscript'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.824
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         11568
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0866
_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^)+(0.1322P)^2^+13.6350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2264
_refine_ls_wR_factor_ref         0.2412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9690
_reflns_number_total             11568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01206a2.cif
_cod_data_source_block           adi-501-ce-c-dipp
_cod_original_cell_volume        3289.78(16)
_cod_database_code               7713153
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ce I C O P '
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.803
_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. Rigid bond restraints
 C49, O20, C50
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C49 \\sim O20 \\sim C50: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Others
 Fixed Sof: H11(0.5) I1A(0.75) I1B(0.25) O19(0.5) C49(0.5) O20(0.5) C50(0.5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10A), C19(H19), C22(H22), C31(H31), C34(H34)
5.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C16(H16), C17(H17A), C27(H27), C28(H28), C29(H29)
5.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)
5.e Idealised tetrahedral OH refined as rotating group:
 O10(H10), O11(H11), O14(H14), O17(H17)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 85 electrons were 
found in a volume of 282\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.2[H2O], 2[CH3OH] per Asymmetric Unit 
which account for 76 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36399
_shelx_fab_checksum              97268
_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 2.058
_oxdiff_exptl_absorpt_empirical_full_min 0.565