A ferric guest inside a spin crossover ferrous helicate
Barrios, Leoní A.; Diego, Rosa; Darawsheh, Mohanad; Martínez, Jesús I.; Roubeau, Oliver; Aromí, Guillem; Chemical Communications  (2022) –; doi:10.1039/D2CC00928E

data_7129969
_publ_section_title
;
 A ferric guest inside a spin crossover ferrous helicate
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00928E
_journal_year                    2022
_chemical_formula_moiety
'C84 H60 Fe2 N18, C6 Fe O12, B F4, 3(C H4 O), 4.75(H2 O)'
_chemical_formula_sum            'C93 H81.5 B F4 Fe3 N18 O19.75'
_chemical_formula_weight         2021.62
_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   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-11-12 deposited with the CCDC.	2022-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.814(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6737(16)
_cell_length_b                   16.6758(13)
_cell_length_c                   28.868(3)
_cell_measurement_reflns_used    9625
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      2.53
_cell_volume                     8910.2(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            220878
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        28.650
_diffrn_reflns_theta_max         28.651
_diffrn_reflns_theta_min         1.469
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             4170
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.530
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1289
_refine_ls_number_reflns         21201
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0742
_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^)+(0.1140P)^2^+22.9177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2172
_refine_ls_wR_factor_ref         0.2214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18591
_reflns_number_total             21201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00928e2.cif
_cod_data_source_block           lp11
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C93 H81.50 B F4 Fe3 N18 O19.75'
_cod_database_code               7129969
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.919
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              49307