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_7713157
_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         'C36 H62 O15 P2 Sm, 1.187(I2), C H4 O, H2 O'
_chemical_formula_sum            'C37 H68 I2.38 O17 P2 Sm'
_chemical_formula_weight         1298.59
_chemical_name_systematic        Sm
_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.cc2fsj5y
_audit_creation_date             2023-03-27
_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                76.591(4)
_cell_angle_beta                 84.307(5)
_cell_angle_gamma                73.542(5)
_cell_formula_units_Z            2
_cell_length_a                   13.0040(8)
_cell_length_b                   13.2938(6)
_cell_length_c                   15.9969(8)
_cell_measurement_reflns_used    24468
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.5760
_cell_measurement_theta_min      2.2930
_cell_volume                     2578.2(2)
_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_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  rigaku
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66179
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.635
_exptl_absorpt_coefficient_mu    2.684
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.61290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)'
_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    1.673
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.775
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         11757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0382P)^2^+10.6931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10281
_reflns_number_total             11757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01206a2.cif
_cod_data_source_block           adi-289-sm
_cod_database_code               7713157
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.689
_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, All O(H,H) groups
2. Others
 Fixed Sof: I2(0.607) I2b(0.05) I3(0.607) I3b(0.02) I2a(0.05) I3a(0.04)
3.a Free rotating group:
 O17(H17A,H17B)
3.b Rotating group:
 O9(H9A,H9B)
3.c Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
3.d Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
3.e Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
3.f Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9C,H9D,H9E), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C37(H37A,H37B,H37C)
3.g Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6), O16(H16A)
;
_shelx_res_checksum              3156
_olex2_exptl_crystal_mounting_method ' '
_olex2_submission_original_sample_id 4_ADI_Sm
_olex2_submission_special_instructions 'No special instructions were received'