Structural elucidation of homometallic anthracenolates synthesised via deprotonative metallation of anthrone.
Clegg, William; Fleming, Ben J.; García-Álvarez, Pablo; Hogg, Lorna M.; Kennedy, Alan R.; Klett, Jan; Martínez-Martínez, Antonio J; Mulvey, Robert E.; Russo, Luca; O'Hara, Charles T; Dalton transactions (Cambridge, England : 2003) 42 (2013) 2512–2519; doi:10.1039/c2dt32176a

data_7022265
_publ_section_title
;
 Structural elucidation of homometallic anthracenolates synthesised via
 deprotonative metallation of anthrone.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2512
_journal_page_last               2519
_journal_paper_doi               10.1039/c2dt32176a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C46 H64 K2 N6 O2'
_chemical_formula_weight         811.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.112(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4500(3)
_cell_length_b                   17.6550(4)
_cell_length_c                   13.5543(4)
_cell_measurement_reflns_used    6390
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.68
_cell_measurement_theta_min      2.80
_cell_volume                     2332.85(12)
_computing_data_collection       CrysalisPro
_computing_molecular_graphics    XSEED
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14911
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5899
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1120
_reflns_number_gt                4025
_reflns_number_total             5899
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2dt32176a.txt
_cod_data_source_block           pgabf1
_cod_original_cell_volume        2332.84(11)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7022265