The crystal structure of (N-([1,1′:4′,1″-terphenyl]-4,4′-diethyl)-2-(bis(pyridin-2-ylmethyl)amino)acetamide-κ 4 N,N,N″, O)tri(nitrato-kO, O′) samarium(III) - methanol - acetonitrile (1/1/1), C40H39SmN8O14
Wang, Hai-Ping; Zhang, Ci-Mao; Huang, Guo-Peng; Liang, Jia-Jun; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 813–815; doi:10.1515/ncrs-2023-0163

data_8107571
_publ_section_title
;
 The crystal structure of
 (N-([1,1&#x2032;:4&#x2032;,1&#x2033;-terphenyl]-4,4&#x2032;-diethyl)-2-(bis(pyridin-2-ylmethyl)amino)acetamide-\k
 4 N,N,N&#x2033;, O)tri(nitrato-kO, O&#x2032;) samarium(III) - methanol -
 acetonitrile (1/1/1), C40H39SmN8O14
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              813
_journal_page_last               815
_journal_paper_doi               10.1515/ncrs-2023-0163
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C38 H36 N7 O14 Sm, C2 H3 N, 1[CH4O]'
_chemical_formula_sum            'C41 H43 N8 O15 Sm'
_chemical_formula_weight         1038.18
_chemical_name_systematic
'(N-([1,1':4',1''-terphenyl]-4,4'-diethyl)-2-(bis(pyridin-2-ylmethyl)amino) acetamide-k4N,N',N'',O)tri(nitrato-kO,O')-Samarium(III) mono acetonitrile"'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                73.549(2)
_cell_angle_beta                 89.1230(10)
_cell_angle_gamma                83.045(2)
_cell_formula_units_Z            2
_cell_length_a                   8.27990(10)
_cell_length_b                   16.6666(5)
_cell_length_c                   17.1471(3)
_cell_measurement_reflns_used    14435
_cell_measurement_temperature    297.71(13)
_cell_measurement_theta_max      76.4600
_cell_measurement_theta_min      4.3620
_cell_volume                     2252.25(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      297.71(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.950
_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   -118.00 -73.00   0.50    1.00    --  -48.38-135.00 152.00   90
  2  \w    -80.00 -55.00   0.50    1.00    --  -48.38 135.00-142.00   50
  3  \w    -88.00 -45.00   0.50    1.00    --  -48.38 135.00  37.00   86
  4  \w   -118.00 -91.00   0.50    1.00    --  -48.38-135.00 -27.00   54
  5  \w     41.00 102.00   0.50    1.00    --   48.38-135.00 152.00  122
  6  \w     40.00  73.00   0.50    1.00    --   48.38-135.00 -27.00   66
  7  \w    -86.00 -55.00   0.50    2.00    --  -91.75 135.00  37.00   62
  8  \w   -119.00 -93.00   0.50    2.00    --  -91.75-135.00 152.00   52
  9  \w    104.00 134.00   0.50    2.00    --  109.06 135.00  37.00   60
 10  \w    148.00 174.00   0.50    2.00    --  109.06 135.00-142.00   52
 11  \w    115.00 144.00   0.50    2.00    --  109.06 135.00-142.00   58
 12  \w     85.00 111.00   0.50    2.00    --  109.06-135.00 -27.00   52
 13  \w     56.00  81.00   0.50    2.00    --  109.06-135.00 152.00   50
 14  \w     46.00  83.00   0.50    2.00    --  109.06-135.00 -27.00   74
 15  \w   -116.00 -60.00   0.50    1.00    --  -48.38 -77.00-120.00  112
 16  \w   -114.00 -77.00   0.50    1.00    --  -48.38-125.00-180.00   74
 17  \w   -120.00 -27.00   0.50    1.00    --  -48.38 -77.00 120.00  186
 18  \w    -99.00 -73.00   0.50    1.00    --  -48.38-125.00  30.00   52
 19  \w    -22.00  27.00   0.50    1.00    --  -48.38  19.00-180.00   98
 20  \w   -161.00-127.00   0.50    2.00    --  -91.75 -57.00  30.00   68
 21  \w   -163.00 -87.00   0.50    2.00    --  -91.75-125.00  30.00  152
 22  \w   -157.00 -79.00   0.50    2.00    --  -91.75 -38.00-150.00  156
 23  \w   -110.00 -80.00   0.50    2.00    --  -91.75 -38.00 150.00   60
 24  \w    -85.00 -19.00   0.50    2.00    --  -91.75 125.00 -90.00  132
 25  \w    -52.00 -19.00   0.50    2.00    --  -91.75  57.00   0.00   66
 26  \w    -65.00 -23.00   0.50    2.00    --  -91.75  57.00-180.00   84
 27  \w   -138.00-113.00   0.50    2.00    --  -91.75-135.00 -27.00   50
 28  \w    -61.00 -24.00   0.50    2.00    --  -91.75 125.00 -60.00   74
 29  \w   -131.00 -78.00   0.50    2.00    --  -91.75 -57.00  60.00  106
 30  \w   -124.00 -80.00   0.50    2.00    --  -91.75 -57.00  30.00   88
 31  \w    -57.00 -32.00   0.50    2.00    --  -91.75  57.00  30.00   50
 32  \w    -77.00 -26.00   0.50    2.00    --  -91.75 125.00-150.00  102
 33  \w    -64.00 -39.00   0.50    2.00    --  -91.75 135.00-142.00   50
 34  \w   -142.00-116.00   0.50    2.00    --  -91.75 -38.00 150.00   52
 35  \w     63.00 103.00   0.50    2.00    --  109.06 -99.00-180.00   80
 36  \w     40.00  66.00   0.50    2.00    --  109.06 -57.00  30.00   52
 37  \w     62.00 100.00   0.50    2.00    --  109.06 -99.00   0.00   76
 38  \w     81.00 110.00   0.50    2.00    --  109.06-125.00   0.00   58
 39  \w     40.00  65.00   0.50    2.00    --  109.06 -57.00 150.00   50
 40  \w     41.00  76.00   0.50    2.00    --  109.06-125.00   0.00   70
 41  \w     39.00  64.00   0.50    2.00    --  109.06 -57.00-150.00   50
 42  \w     38.00  63.00   0.50    2.00    --  109.06 -57.00-180.00   50
 43  \w    110.00 172.00   0.50    2.00    --  109.06  38.00  90.00  124
 44  \w     38.00  63.00   0.50    2.00    --  109.06 -57.00   0.00   50
 45  \w     62.00 105.00   0.50    2.00    --  109.06 -99.00-150.00   86
 46  \w     79.00 106.00   0.50    2.00    --  109.06 -99.00  30.00   54
 47  \w     41.00  68.00   0.50    2.00    --  109.06 -99.00  30.00   54
 48  \w     37.00  62.00   0.50    2.00    --  109.06 -57.00  90.00   50
 49  \w     65.00  92.00   0.50    2.00    --  109.06 -99.00 -90.00   54
 50  \w    104.00 177.00   0.50    2.00    --  109.06  19.00-120.00  146
 51  \w     85.00 110.00   0.50    2.00    --  109.06-125.00-180.00   50
 52  \w     40.00  66.00   0.50    2.00    --  109.06-125.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0003333000
_diffrn_orient_matrix_UB_12      -0.0194759000
_diffrn_orient_matrix_UB_13      0.0933526000
_diffrn_orient_matrix_UB_21      0.0323145000
_diffrn_orient_matrix_UB_22      -0.0950154000
_diffrn_orient_matrix_UB_23      0.0080222000
_diffrn_orient_matrix_UB_31      0.1846709000
_diffrn_orient_matrix_UB_32      0.0046605000
_diffrn_orient_matrix_UB_33      0.0003242000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29937
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.479
_diffrn_reflns_theta_min         4.387
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.448
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       needle
_exptl_crystal_F_000             1054
_exptl_crystal_recrystallization_method 'Acetonitrile, methanol'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.126
_refine_diff_density_min         -2.125
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         8756
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+4.9189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7434
_reflns_number_total             8756
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0163_suppl.cif
_cod_data_source_block           exp_1175_auto
_cod_database_code               8107571
_chemical_oxdiff_formula         'C34 H34 O1 N4 Sm1'
_shelx_estimated_absorpt_t_max   0.367
_shelx_estimated_absorpt_t_min   0.303
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C2-C1
 1.54 with sigma of 0.02
 C23-C24
 1.54 with sigma of 0.02
3. Rigid bond restraints
 O7, N5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O6
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
 N8
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
 C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Sm1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B), C33(H33A,H33B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15),
 C17(H17), C18(H18), C20(H20), C21(H21), C29(H29), C30(H30), C31(H31), C32(H32),
  C35(H35), C36(H36), C37(H37), C38(H38)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C24(H24A,H24B,H24C), C40(H40A,H40B,H40C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 31 electrons were 
found in a volume of 190\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH4O] per Asymmetric Unit 
which account for 36 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84308
_shelx_hkl_checksum              89375
_shelx_fab_checksum              7688
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.046
_oxdiff_exptl_absorpt_empirical_full_min 0.479