α-Tris(2,4-pentanedionato-κ^2^<i>O</i>,<i>O</i>')chromium(III) at 290 and 110K: a new δ phase at 110K
Chrzanowski, Lars S. von; Lutz, Martin; Spek, Anthony L.; Acta Crystallographica Section C 63 (2007) m377–m382; doi:10.1107/S0108270107033823

data_2016085
_publ_section_title
;
 \a-Tris(2,4-pentanedionato-\k^2^<i>O</i>,<i>O</i>')chromium(III) at
 290 and 110K: a new \d phase at 110K
;
_journal_coeditor_code           BG3044
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m377
_journal_page_last               m382
_journal_paper_doi               10.1107/S0108270107033823
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cr (C5 H7 O2)3]'
_chemical_formula_moiety         'C15 H21 Cr O6'
_chemical_formula_sum            'C15 H21 Cr O6'
_chemical_formula_weight         349.32
_chemical_name_systematic
;
\a-Tris(2,4-pentanedionato-\k^2^O,O')chromium(III)
;
_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                 99.2731(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            24
_cell_length_a                   27.5823(2)
_cell_length_b                   7.46560(10)
_cell_length_c                   48.6012(4)
_cell_measurement_reflns_used    117343
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     9877.09(17)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, (1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
;
EVAL14 (set 1) (Duisenberg <i>et al.</i>,  2003), HKL-2000 (set 2)
(Otwinowski
& Minor, 1997) and SORTAV (Blessing, 1987)
;
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'manual editing of SHELXL97 output'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            101596
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1987)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.600
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         18651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                9662
_reflns_number_total             18651
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg3044.cif
_cod_data_source_block           Ib
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2016085
_cod_database_fobs_code          2016085