Molecular Structure of Copper and μ-Oxodiiron Octafluorocorrole Derivatives: Insights into Ligand Noninnocence
Thomas, Kolle E.; Settineri, Nicholas S.; Teat, Simon J.; Steene, Erik; Ghosh, Abhik; ACS Omega  (2020) –; doi:10.1021/acsomega.0c01035

data_4517603
_publ_section_title
;
 Molecular Structure of Copper and \m-Oxodiiron Octafluorocorrole
 Derivatives: Insights into Ligand Noninnocence
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.0c01035
_journal_year                    2020
_chemical_formula_moiety
'C37 H15 Cu F8 N4, 0.71(C H Cl3), 0.14(C H3 O)'
_chemical_formula_sum            'C37.86 H16.14 Cl2.14 Cu F8 N4 O0.14'
_chemical_formula_weight         820.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.819(3)
_cell_angle_gamma                90
_cell_formula_units_Z            28
_cell_length_a                   23.636(2)
_cell_length_b                   34.020(3)
_cell_length_c                   30.888(3)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.4273
_cell_measurement_theta_min      2.1714
_cell_volume                     24218(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 w/PHOTON-II CMOS'
_diffrn_measurement_method       '\w/q shutterless scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            384508
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        21.498
_diffrn_reflns_theta_max         21.498
_diffrn_reflns_theta_min         1.183
_diffrn_source                   'Advanced Light Source beamline 12.2.1'
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       needle
_exptl_crystal_F_000             11476
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.406
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3358
_refine_ls_number_reflns         25642
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0922P)^2^+226.4583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2075
_refine_ls_wR_factor_ref         0.2137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22330
_reflns_number_total             25642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c01035_si_002.cif
_cod_data_source_block           CuF8_TPC_2_a
_cod_original_cell_volume        24218(3)
_cod_database_code               4517603
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.768
_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,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl4) = Uanis(Cl15)
Uanis(O1B) = Uanis(O1A)
3. Rigid body (RIGU) restrains
 Cl5, Cl6, Cl16, C39
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Cl13, Cl14, Cl4, C42
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Others
 Sof(O1A)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(O1B)=Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(1)
 Sof(Cl15)=1-FVAR(2)
 Sof(Cl4)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C38(H38), C42(H42), C39(H39), C41(H41), C40(H40)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28),
 C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
  C21B(H21B), C22B(H22B), C23B(H23B), C24B(H24B), C25B(H25B), C27B(H27B),
 C28B(H28B), C29B(H29B), C30B(H30B), C31B(H31B), C33B(H33B), C34B(H34B),
 C35B(H35B), C36B(H36B), C37B(H37B), C21C(H21C), C22C(H22C), C23C(H23C),
 C24C(H24C), C25C(H25C), C27C(H27C), C28C(H28C), C29C(H29C), C30C(H30C),
 C31C(H31C), C33C(H33C), C34C(H34C), C35C(H35C), C36C(H36C), C37C(H37C),
 C21D(H21D), C22D(H22D), C23D(H23D), C24D(H24D), C25D(H25D), C27D(H27D),
 C28D(H28D), C29D(H29D), C30D(H30D), C31D(H31D), C33D(H33D), C34D(H34D),
 C35D(H35D), C36D(H36D), C37D(H37D), C21E(H21E), C22E(H22E), C23E(H23E),
 C24E(H24E), C25E(H25E), C27E(H27E), C28E(H28E), C29E(H29E), C30E(H30E),
 C31E(H31E), C33E(H33E), C34E(H34E), C35E(H35E), C36E(H36E), C37E(H37E),
 C21F(H21F), C22F(H22F), C23F(H23F), C24F(H24F), C25F(H25F), C27F(H27F),
 C28F(H28F), C29F(H29F), C30F(H30F), C31F(H31F), C33F(H33F), C34F(H34F),
 C35F(H35F), C36F(H36F), C37F(H37F), C21G(H21G), C22G(H22G), C23G(H23G),
 C24G(H24G), C25G(H25G), C27G(H27G), C28G(H28G), C29G(H29G), C30G(H30G),
 C31G(H31G), C33G(H33G), C34G(H34G), C35G(H35G), C36G(H36G), C37G(H37G)
5.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C43(H43D,H43E,H43F)
;
_shelx_res_checksum              20375
_shelx_hkl_checksum              17374
_shelx_fab_checksum              46799
_olex2_submission_special_instructions 'No special instructions were received'