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_7709221
_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 H42 Co F18 N20, 2(B F4), 1.5[CH4O], 0.5[CH4O]'
_chemical_formula_sum            'C62 H50 B2 Co F26 N20 O2'
_chemical_formula_weight         1681.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-11-02
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.10.14 svn.r9718050b for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-11-09 deposited with the CCDC.	2021-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.6857(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.92498(10)
_cell_length_b                   25.4211(2)
_cell_length_c                   23.36412(20)
_cell_measurement_reflns_used    19942
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.7160
_cell_measurement_theta_min      2.5510
_cell_volume                     6981.78(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.22a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.22a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.22a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
'SHELXT 2018/2 (Sheldrick, 2018), intrinsic phasing'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38755
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.342
_diffrn_reflns_theta_min         2.589
_exptl_absorpt_coefficient_mu    3.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.22a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       plate
_exptl_crystal_F_000             3396
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         6686
_refine_ls_number_restraints     332
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0624P)^2^+7.3506P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5988
_reflns_number_total             6686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03535e2.cif
_cod_data_source_block           co_l2_100k_cu
_cod_database_code               7709221
_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. Restrained distances
 B1-F5 \\sim B1-F6 \\sim B1-F7 \\sim B1-F8
 with sigma of 0.02
 F5-F6 \\sim F6-F7 \\sim F7-F8 \\sim F8-F5 \\sim F6-F8 \\sim F5-F7
 with sigma of 0.04
 B1-F6 \\sim B1A-F6A
 with sigma of 0.02
 F5-F7 \\sim F5A-F7A
 with sigma of 0.04
 F7-F8 \\sim F7A-F8A
 with sigma of 0.04
 B1-F7 \\sim B1A-F7A
 with sigma of 0.02
 F6-F7 \\sim F6A-F7A
 with sigma of 0.04
 F5-F6 \\sim F5A-F6A
 with sigma of 0.04
 B1-F5 \\sim B1A-F5A
 with sigma of 0.02
 F5-F8 \\sim F5A-F8A
 with sigma of 0.04
 F6-F8 \\sim F6A-F8A
 with sigma of 0.04
 B1-F8 \\sim B1A-F8A
 with sigma of 0.02
 B2-F9 \\sim B2-F10 \\sim B2-F11 \\sim B2-F12
 with sigma of 0.02
 F9-F10 \\sim F10-F11 \\sim F11-F12 \\sim F12-F9 \\sim F10-F12 \\sim F9-F11
 with sigma of 0.04
 F10-F12 \\sim F10A-F12A
 with sigma of 0.04
 F9-F11 \\sim F9A-F11A
 with sigma of 0.04
 F9-F10 \\sim F9A-F10A
 with sigma of 0.04
 F9-F12 \\sim F9A-F12A
 with sigma of 0.04
 F11-F12 \\sim F11A-F12A
 with sigma of 0.04
 B2-F12 \\sim B2A-F12A
 with sigma of 0.02
 F10-F11 \\sim F10A-F11A
 with sigma of 0.04
 B2-F9 \\sim B2A-F9A
 with sigma of 0.02
 B2-F10 \\sim B2A-F10A
 with sigma of 0.02
 B2-F11 \\sim B2A-F11A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B2 \\sim F9 \\sim F10 \\sim F11 \\sim F12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 B2, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 B2A, F9A, F12A, F11A, F10A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 B1A, F5A, F6A, F7A, F8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 B1, F5, F6, F7, F8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: B1(0.25) F5(0.25) F6(0.25) F7(0.25) F8(0.25) B1A(0.25) F5A(0.25)
 F6A(0.25) F7A(0.25) F8A(0.25) B2(0.25) F9(0.25) F10(0.25) F11(0.25) F12(0.25)
 B2A(0.25) F9A(0.25) F12A(0.25) F11A(0.25) F10A(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C6AA(H6AA,H6AB), C1AA(H1AA,H1AB), C3(H3A,H3B), C0BA(H0BA,H0BB), C9(H9A,H9B),
 C11(H11A,H11B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3BA(H3BA), C4BA(H4BA), C(H), C8(H8), C14(H14), C15(H15), C16(H16),
 C17(H17)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 152 electrons were 
found in a volume of 580\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 1.5[CH4O] in one cavity 
and another 0.5[CH4O] in another cavity per Formula Unit 
which account for 144 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84495
_shelx_fab_checksum              9046
_olex2_submission_special_instructions 'No special instructions were received'