Highly selective and discriminative detection of small alcohols based on a dual-emission macrocyclic samarium complex.
Zhang, Chengjian; Li, Sichen; Zheng, Ruijie; Tai, Shengdi; Yang, Kang; Zhang, Kun; Analytical methods : advancing methods and applications 15 (2023) 361–367; doi:10.1039/d2ay01591a

data_1568031
_publ_section_title
;
 Highly selective and discriminative detection of small alcohols based on
 a dual-emission macrocyclic samarium complex.
;
_journal_issue                   3
_journal_name_full
'Analytical methods : advancing methods and applications'
_journal_page_first              361
_journal_page_last               367
_journal_paper_doi               10.1039/d2ay01591a
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C33 H38 Cl2 N5 O10 Sm, 2(C2 H3 N)'
_chemical_formula_sum            'C37 H44 Cl2 N7 O10 Sm'
_chemical_formula_weight         968.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-06-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.958(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9139(13)
_cell_length_b                   14.0880(11)
_cell_length_c                   17.1758(14)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.406
_cell_measurement_theta_min      2.354
_cell_volume                     4031.0(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52431
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.354
_exptl_absorpt_coefficient_mu    1.654
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0828 before and 0.0658 after correction.
The Ratio of minimum to maximum transmission is 0.9010.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green-yellow
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       block
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.745
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         7944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0220P)^2^+8.3800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6039
_reflns_number_total             7944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ay01591a3.cif
_cod_data_source_block           Sm2l
_cod_depositor_comments          'Adding full bibliography for 1568031.cif.'
_cod_database_code               1568031
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.702
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C29(H29A,H29B), C8(H8A,H8B), C32(H32A,H32B), C7(H7A,H7B),
 C27(H27A,H27B), C31(H31A,H31B), C28(H28A,H28B), C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C26(H26), C21(H21), C11(H11), C5(H5), C3(H3), C13(H13), C33(H33),
 C10(H10), C14(H14)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              44786
_shelx_hkl_checksum              4923
_olex2_submission_special_instructions 'No special instructions were received'