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_7701426
_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 Ga2 O18, 4(C4 H8 O)'
_chemical_formula_sum            'C88 H80 Ga2 O22'
_chemical_formula_weight         1628.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-23 deposited with the CCDC.    2019-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.915(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3656(6)
_cell_length_b                   23.5579(9)
_cell_length_c                   19.8257(8)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.68
_cell_measurement_theta_min      2.47
_cell_volume                     7615.5(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.6
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32008
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.799
_diffrn_reflns_theta_min         3.094
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0895 before and 0.0420 after correction.
The Ratio of minimum to maximum transmission is 0.9006.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       block
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.165
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         8081
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0484P)^2^+20.6264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6993
_reflns_number_total             8081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03398j2.cif
_cod_data_source_block           1679_da2_0m
_cod_database_code               7701426
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O9-H9
 0.9 with sigma of 0.02
 O4-H4
 0.9 with sigma of 0.02
 O1-H1
 0.9 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C42(H42A,H42B), C43(H43A,H43B), C38(H38A,H38B), C41(H41A,
 H41B), C12(H12A,H12B), C40(H40A,H40B), C44(H44A,H44B)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C0AA(H0AA), C30(H30), C13(H13), C28(H28), C26(H26), C8(H8),
 C24(H24), C25(H25), C5(H5), C33(H33), C17(H17), C21(H21), C3(H3), C2(H2),
 C18(H18), C4(H4A), C15(H15), C16(H16), C36(H36), C35(H35), C34(H34)
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_shelx_res_checksum              88422
_olex2_submission_special_instructions 'No special instructions were received'