Diaquatris(pentane-2,4-dionato-<i>O</i>,<i>O</i>')holmium(III) monohydrate and diaquatris(pentane-2,4-dionato-<i>O</i>,<i>O</i>')holmium(III) 4-hydroxypentan-2-one solvate dihydrate
Kooijman, Huub; Nijsen, Frank; Spek, Anthony L.; Schip, Fred van het; Acta Crystallographica Section C 56 (2000) 156–158; doi:10.1107/S0108270199013566

data_2010602
_publ_section_title
;
 Diaquatris(pentane-2,4-dionato-<i>O</i>,<i>O</i>')holmium(III)
 monohydrate and
 diaquatris(pentane-2,4-dionato-<i>O</i>,<i>O</i>')holmium(III)
 4-hydroxypentan-2-one solvate dihydrate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              156
_journal_page_last               158
_journal_paper_doi               10.1107/S0108270199013566
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Ho (C5 H7 O2)3 (H2 O)2] , C5 H8 O2 , H2 O'
_chemical_formula_moiety         'C15 H25 Ho O8 , C5 H8 O2 , 2H2 O'
_chemical_formula_sum            'C20 H37 Ho O12'
_chemical_formula_weight         634.43
_chemical_name_systematic
;diaquatris(pentane-2,4-dionato-O,O')holmium(III) 4-hydroxypentan-2-one
 solvate
dihydrate
;
_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'
_cell_angle_alpha                90
_cell_angle_beta                 93.440(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4903(11)
_cell_length_b                   11.0242(6)
_cell_length_c                   20.5442(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      18.35
_cell_measurement_theta_min      11.49
_cell_volume                     2597.7(3)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection
'locally modified CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4T'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .041
_diffrn_reflns_av_sigmaI/netI    .047
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9388
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.10
_exptl_absorpt_correction_T_max  .857
_exptl_absorpt_correction_T_min  .517
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(Spek, 1990)'
_exptl_crystal_colour            yellow-pink
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          .70
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .05
_refine_diff_density_max         1.66
_refine_diff_density_min         -1.96
_refine_ls_abs_structure_details none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4697
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          .043
_refine_ls_R_factor_gt           .032
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(F~o^~2^)+(0.02P)^2^+5P] where P=(F~o~^2^+2F~c~^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .069
_reflns_number_gt                3764
_reflns_number_total             4697
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1374.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian'
changed to 'gaussian' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2010602
_cod_database_fobs_code          2010602