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_7701428
_publ_section_title
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 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_moiety         'C72 H48 Ga2 O15'
_chemical_formula_sum            'C72 H48 Ga2 O15'
_chemical_formula_weight         1292.54
_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
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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                 127.401(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.064(3)
_cell_length_b                   17.699(2)
_cell_length_c                   18.156(4)
_cell_measurement_reflns_used    2403
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.88
_cell_measurement_theta_min      2.30
_cell_volume                     5887.7(18)
_computing_cell_refinement       'SAINT (Bruker)'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'SAINT (Bruker)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II QUAZAR'
_diffrn_measurement_method       '\f and \w rotation with narrow frames'
_diffrn_radiation_source         'multilayer monochromator ImuS'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.0905
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14077
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        18.845
_diffrn_reflns_theta_max         18.847
_diffrn_reflns_theta_min         2.300
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       plate
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
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_refine_ls_abs_structure_Flack   0.48(10)
_refine_ls_extinction_coef       0.0029(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         4579
_refine_ls_number_restraints     1317
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1315
_refine_ls_R_factor_gt           0.0927
_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^)+(0.0638P)^2^+169.4421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2169
_refine_ls_wR_factor_ref         0.2399
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                3237
_reflns_number_total             4579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03398j2.cif
_cod_data_source_block           1700_RR18
_cod_original_cell_volume        5887.7(17)
_cod_database_code               7701428
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              79293