Tris{<i>N</i>-[bis(dimethylamino)phosphinoyl]-2,2,2-trichloroacetamido}(triphenylphosphine oxide)holmium(III)
Amirkhanov, Oleksiy V.; Marchenko, Ivan O.; Moroz, Olesia V.; Sliva, Tetyana Yu.; Fritsky, Igor O.; Acta Crystallographica Section E 66 (2010) m640–m641; doi:10.1107/S160053681001665X

data_2226087
_publ_section_title
;
 Tris{<i>N</i>-[bis(dimethylamino)phosphinoyl]-2,2,2-trichloroacetamido}(triphenylphosphine
 oxide)holmium(III)
;
_journal_coeditor_code           CV2713
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m640
_journal_page_last               m641
_journal_paper_doi               10.1107/S160053681001665X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Ho (C6 H12 Cl3 N3 O2 P)3 (C18 H15 O P)]'
_chemical_formula_moiety         'C36 H51 Cl9 Ho N9 O7 P4'
_chemical_formula_sum            'C36 H51 Cl9 Ho N9 O7 P4'
_chemical_formula_weight         1329.72
_chemical_name_systematic
;
Tris{<i>N</i>-[bis(dimethylamino)phosphinoyl]-2,2,2-
trichloroacetamido}(triphenylphosphine oxide)holmium(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                 120.462(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1338(4)
_cell_length_b                   23.2403(9)
_cell_length_c                   23.6071(8)
_cell_measurement_reflns_used    24428
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.75
_cell_volume                     5738.1(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24428
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.958
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.761
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         10386
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0588P)^2^+5.5377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                7799
_reflns_number_total             10386
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2713.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2226087
_cod_database_fobs_code          2226087