Solid-state and solution-phase characterization of Sm<sup>II</sup>-aza[2.2.2]cryptate and its methylated analogue.
Bokouende, Sergely Steephen; Jenks, Tyler C.; Ward, Cassandra L.; Allen, Matthew J.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 10852–10855; doi:10.1039/d2dt01823c

data_7710808
_publ_section_title
;
 Solid-state and solution-phase characterization of
 Sm<sup>II</sup>-aza[2.2.2]cryptate and its methylated analogue.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10852
_journal_page_last               10855
_journal_paper_doi               10.1039/d2dt01823c
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C18 H42 I N8 Sm, I'
_chemical_formula_sum            'C18 H42 I2 N8 Sm'
_chemical_formula_weight         774.74
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-03-28 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7551(9)
_cell_length_b                   12.1307(7)
_cell_length_c                   13.7979(8)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.85
_cell_measurement_theta_min      2.58
_cell_volume                     2637.1(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      100
_diffrn_detector                 'Photon III'
_diffrn_detector_type            'CPAD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.8 mm pinhole collimator'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51941
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.237
_diffrn_reflns_theta_min         2.119
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.588
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0881 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.7589.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_description       plate
_exptl_crystal_F_000             1496
_exptl_crystal_recrystallization_method
'vapor diffusion of THF into acetonitrile'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details
;
 Flack x determined using 2957 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         9830
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0262P)^2^+1.2838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                7976
_reflns_number_total             9830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01823c2.cif
_cod_data_source_block           mja_ssb_4_51
_cod_database_code               7710808
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.657
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N5(H5), N8(H8), N6(H6), N7(H7), N3(H3), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C8(H8A,H8B), C1(H1A,H1B), C18(H18A,H18B), C6(H6A,H6B), C3(H3A,
 H3B), C11(H11A,H11B), C9(H9A,H9B), C10(H10A,H10B), C7(H7A,H7B), C17(H17A,H17B),
  C15(H15A,H15B), C16(H16A,H16B), C13(H13A,H13B), C4(H4A,H4B), C12(H12A,H12B),
 C14(H14A,H14B), C2(H2A,H2B)
;
_shelx_res_checksum              18991
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MicroMount (MiTeGen) with polyfluoroether oil (Fomblin YR-1800, Alfa Aesar)'
_olex2_submission_special_instructions 'No special instructions were received'