Self-assembly of a trigonal bipyramidal architecture with stabilisation of iron in three spin states.
Taylor, Lauren L. K.; Vitorica-Yrezabal, Iñigo J; Borilović, Ivana; Tuna, Floriana; Riddell, Imogen A.; Chemical communications (Cambridge, England) 57 (2021) 11252–11255; doi:10.1039/d1cc04413c

data_7129108
_publ_section_title
;
 Self-assembly of a trigonal bipyramidal architecture with stabilisation
 of iron in three spin states.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11252
_journal_page_last               11255
_journal_paper_doi               10.1039/d1cc04413c
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C20.63 H19.53 Br0.05 N3.95 O1.91'
_chemical_formula_sum            'C20.62 H19.53 Br0.05 N3.96 O1.9'
_chemical_formula_weight         356.88
_chemical_name_systematic        AIR3
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-09 deposited with the CCDC.	2021-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                75.420(14)
_cell_angle_beta                 86.542(13)
_cell_angle_gamma                79.753(14)
_cell_formula_units_Z            2
_cell_length_a                   8.3959(14)
_cell_length_b                   10.4913(17)
_cell_length_c                   10.5635(18)
_cell_measurement_reflns_used    1526
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      26.7950
_cell_measurement_theta_min      3.1320
_cell_volume                     886.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -11.00  90.00   1.00    7.50    --   20.02  77.00  30.00  101
  2  \w    -10.00  90.00   1.00    7.50    --   20.02  77.00 150.00  100
  3  \w    -10.00  90.00   1.00    7.50    --   20.02  77.00 -90.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0053209000
_diffrn_orient_matrix_UB_12      0.0668469000
_diffrn_orient_matrix_UB_13      -0.0005011000
_diffrn_orient_matrix_UB_21      -0.0854914000
_diffrn_orient_matrix_UB_22      0.0148828000
_diffrn_orient_matrix_UB_23      0.0059034000
_diffrn_orient_matrix_UB_31      0.0059320000
_diffrn_orient_matrix_UB_32      -0.0182390000
_diffrn_orient_matrix_UB_33      0.0691367000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0907
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4679
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.921
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_preparation       'In chloroform'
_exptl_crystal_recrystallization_method 'Slow evaporation of cloroform'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3224
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0797
_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^)+(0.1060P)^2^+0.2780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1992
_refine_ls_wR_factor_ref         0.2417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2028
_reflns_number_total             3224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04413c2.cif
_cod_data_source_block           air3
_cod_depositor_comments
'Adding full bibliography for 7129106--7129112.cif.'
_cod_original_formula_sum        'C20.62 H19.53 Br0.05 N3.96 O1.90'
_cod_database_code               7129108
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C19 H14 N4 O'
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.963
_reflns_odcompleteness_completeness 98.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Br0 \\sim C008: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Others
 Sof(Br0)=1-FVAR(1)
 Sof(O001)=Sof(O002)=Sof(C008)=Sof(C00K)=Sof(H00K)=Sof(C00N)=Sof(H00N)=
 Sof(C00E)=Sof(N003)=Sof(C007)=Sof(H007)=Sof(C00I)=Sof(H00I)=Sof(C00L)=
 Sof(H00A)=Sof(H00B)=Sof(H00D)=Sof(C00P)=Sof(H00E)=Sof(H00F)=Sof(H00L)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C00I(H00I)
4.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00N(H00N), C007(H007), C00C(H00C), C00G(H00G), C00H(H00H),
 C00J(H00J), C00M(H00M), C00O(H00O), C00Q(H00Q)
4.c Fitted hexagon refined as free rotating group:
 C008(C00K,C00N,C00E,N003,C007)
4.d Idealised Me refined as rotating group:
 C00L(H00A,H00B,H00D), C00P(H00E,H00F,H00L), C00R(H00P,H00R,H00S)
;
_shelx_res_checksum              90917
_shelx_hkl_checksum              22532
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.664
_oxdiff_exptl_absorpt_empirical_full_min 0.736