On the structure refinement of metal complexes against 3D electron diffraction data using multipolar scattering factors.
Pacoste, Laura; Ignat'ev, Vladislav Mikhailovich; Dominiak, Paulina Maria; Zou, Xiaodong; IUCrJ 11 (2024) –; doi:10.1107/S2052252524006730

data_1572371
_publ_section_title
;
 On the structure refinement of metal complexes against 3D electron
 diffraction data using multipolar scattering factors.
;
_journal_issue                   5
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524006730
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C15 H21 Fe O6'
_chemical_formula_sum            'C15 H21 Fe O6'
_chemical_formula_weight         353.175
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_audit_creation_date             2024-04-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.190(3)
_cell_length_b                   13.390(3)
_cell_length_c                   16.369(3)
_cell_measurement_reflns_used    9267
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.90
_cell_measurement_theta_min      2.70
_cell_volume                     3329.4(12)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.04
_diffrn_measured_fraction_theta_full 0.9968
_diffrn_measured_fraction_theta_max 0.9968
_diffrn_measurement_device_type  'Bruker SMART CCD Apex-II area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.9877
_diffrn_reflns_Laue_measured_fraction_max 0.9616
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30371
_diffrn_reflns_point_group_measured_fraction_full 0.9968
_diffrn_reflns_point_group_measured_fraction_max 0.9968
_diffrn_reflns_theta_full        65.0831
_diffrn_reflns_theta_max         65.08
_diffrn_reflns_theta_min         5.17
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.493
_exptl_absorpt_correction_T_max  0.433
_exptl_absorpt_correction_T_min  0.104
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             1477.249
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.2958
_refine_diff_density_min         -0.3151
_refine_diff_density_rms         0.0534
_refine_ls_d_res_high            0.8500
_refine_ls_d_res_low             8.5610
_refine_ls_extinction_coef       0.00074(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0413
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     206
_refine_ls_number_reflns         2821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0413
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+2.2044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2611
_reflns_number_total             2821
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            jf5002.cif
_cod_data_source_block           XRD_IAM_neutral
_cod_original_cell_volume        3329.1(12)
_cod_database_code               1572371
_shelx_estimated_absorpt_t_min   0.102
_shelx_estimated_absorpt_t_max   0.373
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C010(H010), C012(H012), C013(H013)
2.b Idealised Me refined as rotating group:
 C007(H00a,H00b,H00c), C008(H00d,H00e,H00f), C009(H00g,H00h,H00i), C011(H01a,
 H01b,H01c), C014(H01d,H01e,H01f), C015(H01g,H01h,H01i)
;
_olex2_submission_special_instructions 'No special instructions were received'