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_7710807
_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         'C24 H54 N8 Sm, 2(I), 2(C2 H3 N)'
_chemical_formula_sum            'C28 H60 I2 N10 Sm'
_chemical_formula_weight         941.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-09 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                   19.4034(11)
_cell_length_b                   18.0204(10)
_cell_length_c                   10.3393(6)
_cell_measurement_reflns_used    7534
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      2.26
_cell_volume                     3615.2(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32079
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.449
_diffrn_reflns_theta_min         2.099
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.365
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0865 before and 0.0605 after correction. The Ratio of minimum to maximum transmission is 0.8047. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       plate
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 1460 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3724
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0150P)^2^+5.3151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0463
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3322
_reflns_number_total             3724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01823c2.cif
_cod_data_source_block           tj_sm_aba2
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7710807
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.669
_shelx_estimated_absorpt_t_min   0.332
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B), C4(H4A,H4B), C11(H11A,H11B), C8(H8A,
 H8B), C10(H10A,H10B), C5(H5A,H5B), C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              91066
_olex2_submission_special_instructions 'No special instructions were received'