The crystal structure of diaqua-tris(nitrato-κ2 O,O′)-bis(4,4,5,5-tetramethyl-2-(p-pyridyl)imidazoline-1-oxyl 3-oxide-κN)samarium(III), C24H36N9O15Sm
Li, Dongjiao; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1463–1464; doi:10.1515/ncrs-2020-0359

data_8105495
_publ_section_title
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 The crystal structure of diaqua-tris(nitrato-\k2
 O,O&#x2032;)-bis(4,4,5,5-tetramethyl-2-(p-pyridyl)imidazoline-1-oxyl
 3-oxide-\kN)samarium(III), C24H36N9O15Sm
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_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1463
_journal_page_last               1464
_journal_paper_doi               10.1515/ncrs-2020-0359
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C24 H36 N9 O15 Sm'
_chemical_formula_sum            'C24 H36 N9 O15 Sm'
_chemical_formula_weight         840.97
_chemical_name_systematic
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 The crystal structure of diaqua-tris(nitrato-\k^2^<i>O</i>,<i>O</i>')
-bis(4,4,5,5-tetramethyl-2-(<i>p</i>-pyridyl)imidazoline-1-oxyl
 3-oxide-\k<i>N</i>)samarium(III), C~24~H~36~N~9~O~15~Sm

;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 94.6460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.625(3)
_cell_length_b                   11.6837(12)
_cell_length_c                   11.9293(12)
_cell_measurement_reflns_used    5073
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.55
_cell_volume                     3282.0(6)
_computing_cell_refinement       'Bruker SMART APEX II [1]'
_computing_data_collection       'Bruker SMART APEX II [1]'
_computing_data_reduction        'Bruker SAINT [2]'
_computing_molecular_graphics    'Olex2 [3]'
_computing_publication_material  'Olex2 [3]'
_computing_structure_refinement  'ShelXL [4]'
_computing_structure_solution    'XS [5]'
_diffrn_ambient_temperature      293.15
_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  0.0191
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8697
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.029
_diffrn_reflns_theta_max         25.029
_diffrn_reflns_theta_min         1.946
_diffrn_source                   '(Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.872
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.775574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2911
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+1.8605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0449
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2726
_reflns_number_total             2911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0359_suppl.cif
_cod_data_source_block           50329a
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'NONE' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
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_cod_original_cell_volume        3281.9(6)
_cod_database_code               8105495
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H8A-H8B
 1.45 with sigma of 0.01
 O8-H8A = O8-H8B
 0.85 with sigma of 0.001
3.a Riding coordinates:
 O8(H8A,H8B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
3.c Idealised Me refined as rotating group:
 C8(H8C,H8D,H8E), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;