Designed Asymmetric Coordination Helicates with bis-β-diketonate Ligands
Aromi, Guillem; Darawsheh, Mohanad; Diego, Rosa; Barrios, Leoní Alejandra; Sadurní, Anna; Garcia Gomez, Jordi; Lloyd, Paul; Teat, Simon; Roubeau, Olivier; Aguilà, David; Dalton Transactions  (2019) –; doi:10.1039/C9DT03398J

data_7701427
_publ_section_title
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 Designed Asymmetric Coordination Helicates with bis-\b-diketonate Ligands
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03398J
_journal_year                    2019
_chemical_formula_moiety         'C72 H48 Fe2 O15'
_chemical_formula_sum            'C72 H48 Fe2 O15'
_chemical_formula_weight         1264.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-05-23 deposited with the CCDC.    2019-10-23 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 127.106(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.111(7)
_cell_length_b                   17.662(6)
_cell_length_c                   18.343(5)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.28
_cell_measurement_theta_min      2.75
_cell_volume                     5971(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\p and \w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38712
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        28.965
_diffrn_reflns_theta_max         28.967
_diffrn_reflns_theta_min         2.515
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
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 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12040
_refine_ls_number_restraints     1504
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0898
_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^)+(0.0514P)^2^+71.2126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2225
_refine_ls_wR_factor_ref         0.2401
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                9121
_reflns_number_total             12040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03398j2.cif
_cod_data_source_block           md245_Cc
_cod_database_code               7701427
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.940
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              11231