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_7701425
_publ_section_title
;
 Designed Asymmetric Coordination Helicates with bis-\b-diketonate Ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03398J
_journal_year                    2019
_chemical_formula_sum            'C85 H74.33 Fe2 O21.25'
_chemical_formula_weight         1547.47
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-05-23 deposited with the CCDC.    2019-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.815(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   23.4757(17)
_cell_length_b                   34.645(2)
_cell_length_c                   30.737(2)
_cell_measurement_reflns_used    9463
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.48
_cell_volume                     24053(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.881
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            324922
_diffrn_reflns_point_group_measured_fraction_full 0.881
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         26.514
_diffrn_reflns_theta_min         1.282
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6309
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       Needle
_exptl_crystal_F_000             9676
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.383
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3134
_refine_ls_number_reflns         38337
_refine_ls_number_restraints     1209
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1401P)^2^+30.4627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30367
_reflns_number_total             38337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03398j2.cif
_cod_data_source_block           cs571
_cod_database_code               7701425
_shelx_estimated_absorpt_t_min   0.812
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2013-4
_shelx_res_checksum              55924