A large axial magnetic anisotropy in trigonal bipyramidal Fe(ii).
Hay, Moya A.; Sarkar, Arup; Craig, Gavin A.; Marriott, Katie E. R.; Wilson, Claire; Rajaraman, Gopalan; Murrie, Mark; Chemical communications (Cambridge, England) 56 (2020) 6826–6829; doi:10.1039/d0cc02382e

data_7126496
_publ_section_title
;
 A large axial magnetic anisotropy in trigonal bipyramidal Fe(ii).
;
_journal_issue                   50
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6826
_journal_page_last               6829
_journal_paper_doi               10.1039/d0cc02382e
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C14 H30 Cl3 Fe N4, Cl O4'
_chemical_formula_sum            'C14 H30 Cl4 Fe N4 O4'
_chemical_formula_weight         516.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-03-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-03-23 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.504(3)
_cell_length_b                   12.830(3)
_cell_length_c                   13.185(3)
_cell_measurement_reflns_used    3625
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.02
_cell_measurement_theta_min      2.27
_cell_volume                     2115.2(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'charge integrating pixel array detector'
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1208
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.718
_diffrn_reflns_theta_min         1.587
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.246
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1297 before and 0.1078 after correction. The Ratio of minimum to maximum transmission is 0.7817. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4010
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0316P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                2952
_reflns_number_total             4010
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02382e2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7126496.cif.'
_cod_original_cell_volume        2115.3(8)
_cod_database_code               7126496
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.99(4)
 0.01(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C2A(H2Aa,H2Ab), C2C(H2Ca,H2Cb), C4C(H4Ca,H4Cb), C1A(H1Aa,H1Ab), C4B(H4Ba,
 H4Bb), C1B(H1Ba,H1Bb), C2B(H2Ba,H2Bb), C4A(H4Aa,H4Ab), C3B(H3Ba,H3Bb),
 C3C(H3Ca,H3Cb), C1C(H1Ca,H1Cb), C3A(H3Aa,H3Ab)
3.b Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C5(H5a,H5b,H5c)
;
_olex2_submission_special_instructions 'No special instructions were received'