Crystal structure and Hirshfeld surface analysis of ((<i>S</i>,<i>S</i>)-2,2'-{[(1,2-diphenylethane-1,2-diyl)bis[(azaniumylylidene)methanylylidene]}bis(6-methoxyphenolato))trinitratosamarium(III)
Okumura, Yuta; Takiguchi, Yuji; Nakane, Daisuke; Akitsu, Takashiro; Acta Crystallographica Section E 77 (2021) 579–582; doi:10.1107/S2056989021004424

data_2243821
_publ_section_title
;
 Crystal structure and Hirshfeld surface analysis of
 ((<i>S</i>,<i>S</i>)-2,2'-{[(1,2-diphenylethane-1,2-diyl)bis[(azaniumylylidene)methanylylidene]}bis(6-methoxyphenolato))trinitratosamarium(III)
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              579
_journal_page_last               582
_journal_paper_doi               10.1107/S2056989021004424
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration syn
_chemical_formula_iupac          '[Sm (N O3)3 (C30 H28 N2 O4)]'
_chemical_formula_moiety         'C30 H28 N5 O13 Sm'
_chemical_formula_sum            'C30 H28 N5 O13 Sm'
_chemical_formula_weight         816.92
_chemical_name_systematic
((<i>S</i>,<i>S</i>)-2,2'-{(1,2-diphenylethane-1,2-diyl)bis[(azaniumylylidene)methanylylidene]}bis(6-methoxyphenolato))trinitratosamarium(III)
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 98.7270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.9105(6)
_cell_length_b                   15.7993(5)
_cell_length_c                   21.5738(7)
_cell_measurement_reflns_used    859
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.6272
_cell_measurement_theta_min      1.7046
_cell_volume                     6371.0(4)
_computing_cell_refinement
;
APEX3 (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
<i>shelXle</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.812
_diffrn_measurement_device_type  'Bruker APEXIII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40695
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.338
_diffrn_reflns_theta_min         1.910
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.919
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.297
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.840
_refine_diff_density_min         -1.577
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4865 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.009(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         15028
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.847
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0334
_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^)+(0.1000P)^2^+0.6514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                12523
_reflns_number_total             15028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2039sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2243821
_cod_database_fobs_code          2243821
_shelx_estimated_absorpt_t_min   0.397
_shelx_estimated_absorpt_t_max   0.828
_shelx_hkl_checksum              36898
_shelx_res_checksum              55694