Spin-state control of cobalt(II) and iron(II) complexes with click-derived tripodal ligands through non-covalent and fluorine-specific interactions.
Nößler, Maite; Hunger, David; Reichert, Felix; Winkler, Mario; Reimann, Marc; Klein, Johannes; Suhr, Simon; Suntrup, Lisa; Beerhues, Julia; Kaupp, Martin; van Slageren, Joris; Sarkar, Biprajit; Dalton transactions (Cambridge, England : 2003) 50 (2021) 18097–18106; doi:10.1039/d1dt03535e

data_7709222
_publ_section_title
;
 Spin-state control of cobalt(II) and iron(II) complexes with
 click-derived tripodal ligands through non-covalent and fluorine-specific
 interactions.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18097
_journal_page_last               18106
_journal_paper_doi               10.1039/d1dt03535e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C60 H30 F30 Fe N20, 2(B F4)'
_chemical_formula_sum            'C60 H30 B2 F38 Fe N20'
_chemical_formula_weight         1830.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-11-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-11-09 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.545(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.2429(9)
_cell_length_b                   9.3972(5)
_cell_length_c                   24.0242(12)
_cell_measurement_reflns_used    4691
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.423
_cell_measurement_theta_min      2.339
_cell_volume                     3532.9(3)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT+ (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'omega + phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40698
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.423
_diffrn_reflns_theta_min         2.339
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.710
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         6497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.710
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0640
_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^)+(0.1638P)^2^+33.1774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1843
_refine_ls_wR_factor_ref         0.2179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4691
_reflns_number_total             6497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03535e2.cif
_cod_data_source_block           bip522_a
_cod_database_code               7709222
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C13(H13a,H13b), C20(H20a,H20b), C30(H30a,H30b), C23(H23a,
 H23b), C33(H33a,H33b)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C22(H22), C32(H32)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 72 electrons were 
found in a volume of 268\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[CH4O] per Formula Unit 
which account for 72 electrons per unit cell.
;
_shelx_res_checksum              71235
_shelx_fab_checksum              10185
_olex2_submission_special_instructions 'No special instructions were received'