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_7713154
_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
'0.5(C36 H57 Eu O15 P2), 0.5(C36 H62 Eu O15 P2), I3, 0.5(H2 O), 0.5(C2 H3 O), O'
_chemical_formula_sum            'C37 H62 Eu I3 O17 P2'
_chemical_formula_weight         1373.46
_chemical_name_systematic        1
_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     direct
_audit_block_doi                 10.5517/ccdc.csd.cc2fsj6z
_audit_creation_date             2023-03-28
_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                89.081(3)
_cell_angle_beta                 89.653(3)
_cell_angle_gamma                85.828(3)
_cell_formula_units_Z            4
_cell_length_a                   12.5932(6)
_cell_length_b                   16.6149(5)
_cell_length_c                   25.0246(9)
_cell_measurement_reflns_used    6713
_cell_measurement_temperature    100
_cell_measurement_theta_max      19.8850
_cell_measurement_theta_min      2.4560
_cell_volume                     5221.4(3)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_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   -104.00  19.00   1.00    6.00    --  -14.30 -39.00-169.00  123
  2  \w   -104.00  19.00   1.00    6.00    --  -14.30 -38.00  30.00  123
  3  \w    -53.00  75.00   1.00    6.00    --  -14.30  72.00 120.00  128
  4  \w    -48.00  75.00   1.00    6.00    --  -14.30  39.00 -15.00  123
  5  \w   -104.00  24.00   1.00    6.00    --  -14.30 -72.00   0.00  128
  6  \w    -53.00  13.00   1.00    6.00    --  -14.30  72.00   0.00   66
  7  \w    -53.00  75.00   1.00    6.00    --  -14.30  72.00-180.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1362
_diffrn_reflns_av_unetI/netI     0.1214
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            90519
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.621
_exptl_absorpt_coefficient_mu    3.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54621
_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    1.747
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_preparation       0
_exptl_crystal_recrystallization_method 00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.944
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1127
_refine_ls_number_reflns         18292
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1557
_refine_ls_R_factor_gt           0.1008
_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^)+(0.0839P)^2^+70.1595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2028
_refine_ls_wR_factor_ref         0.2410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11692
_reflns_number_total             18292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01206a2.cif
_cod_data_source_block           adi-393-eu-crown-dipp
_cod_database_code               7713154
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.0006(2)
 -0.0006(2)
2. 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
3. Restrained distances
 Eu2-H20A \\sim Eu2-H20B
 with sigma of 0.02
 Eu1-H5A \\sim Eu1-H5B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C53) \\sim Ueq: with sigma of 0.051 and sigma for terminal atoms of 0.05
Uanis(C8A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C8B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: I6A(0.8) I6B(0.2) C8A(0.4) C8B(0.6) C74(0.5) H74A(0.5) H74B(0.5)
 H74C(0.5) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5)
6.a Free rotating group:
 O5(H5A,H5B), O20(H20A,H20B), O32(H32A,H32B)
6.b Ternary CH refined with riding coordinates:
 C10(H10), C34(H34), C43(H43), C46(H46), C67(H67), C70(H70), C77(H77)
6.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20C,H20D), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
  C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,
 H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C5(H5), C18(H18), C30(H30), C31(H31), C32(H32), C39(H39),
 C40(H40), C41(H41), C63(H63), C64(H64), C65(H65)
6.e Fitted hexagon refined as free rotating group:
 C33(C28,C29,C30,C31,C32)
6.f Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C),
 C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C76(H76A,H76B,H76C), C78(H78A,H78B,
 H78C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C)
6.g Idealised tetrahedral OH refined as rotating group:
 O4(H4), O7(H7), O19(H19), O28(H28)
;
_shelx_res_checksum              31976
_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
;