Crystal structure of tetra[bis(diphenylphosphino)methane dioxide-O,O']dysprosium(III) tri(trifluoromethanesulfonate) — N,N'-dimethylformamide (1:2), [Dy(C25H22P2O2)4][CF3SO3]3 · 2C3H7NO
Qiong-Hua Jin; Jie-Qiang Wu; Yuan-Yuan Zhang; Cun-Lin Zhang; Zeitschrift für Kristallographie - New Crystal Structures 224 (2009) 428–; doi:

data_8102462
_publ_section_title
;
 Crystal structure of tetra[bis(diphenylphosphino)methane
 dioxide-O,O']dysprosium(III) tri(trifluoromethanesulfonate) ---
 N,N'-dimethylformamide (1:2), [Dy(C25H22P2O2)4][CF3SO3]3 &#x00B7;
 2C3H7NO
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              428
_journal_volume                  224
_journal_year                    2009
_chemical_formula_sum            'C109 H102 Dy F9 N2 O19 P8 S3'
_chemical_formula_weight         2421.37
_chemical_name_systematic
; 
 Crystal structure of {tetra[bis(diphenylphosphino)
methane dioxide-O,O']dysprosium(III) 
trifluoromethanesulfonate-N,N'-dimethylformamide(1:2)},
[Dy(dppmo~2~)~4~](OTf)~3~.2DMF 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.076(2)
_cell_angle_beta                 83.9880(10)
_cell_angle_gamma                65.5750(10)
_cell_formula_units_Z            2
_cell_length_a                   15.8588(13)
_cell_length_b                   18.6305(17)
_cell_length_c                   20.687(2)
_cell_measurement_reflns_used    9049
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.845
_cell_measurement_theta_min      2.204
_cell_volume                     5534.2(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29021
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.6798
_exptl_absorpt_correction_T_min  0.6537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2474
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.45
_refine_diff_density_max         1.521
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1419
_refine_ls_number_reflns         19225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+15.8312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                13912
_reflns_number_total             19225
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2644.cff
_cod_data_source_block           081205c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

'_geom_bond_publ_flag' value 'N' changed to 'n' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (266
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (28
times).

'_geom_angle_publ_flag' value 'N' changed to 'n' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (454 times).

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

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_cell_volume        5534.3(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8102462