Stabilization of the previously unknown tautomer HP(OH)2 of hypophosphorous acid as ligand; preparation of [W3(Ni(HP(OH)2))Q4(H2O)9]4+(Q = S, Se) complexes
Sokolov, Maxim N.; Hernández-Molina, Rita; Clegg, William; Fedin, Vladimir P.; Mederos, Alfredo; Chemical Communications  (2003) 140–141; doi:10.1039/b209792c

data_7113905
_publ_section_title
;
 Stabilization of the previously unknown tautomer HP(OH)2 of
 hypophosphorous acid as ligand; preparation of
 [W3(Ni(HP(OH)2))Q4(H2O)9]4+(Q = S, Se) complexes
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              140
_journal_page_last               141
_journal_paper_doi               10.1039/b209792c
_journal_year                    2003
_chemical_formula_sum            'C36 H77 Cl4 N24 Ni O34 P Se4 W3'
_chemical_formula_weight         2489.09
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.391(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.5728(5)
_cell_length_b                   18.5868(6)
_cell_length_c                   48.7091(16)
_cell_measurement_reflns_used    42315
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.57
_cell_measurement_theta_min      2.21
_cell_volume                     14803.0(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            62151
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.132
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.209
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             9616
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.614
_refine_diff_density_min         -5.188
_refine_diff_density_rms         0.283
_refine_ls_extinction_coef       0.000038(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         17547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.633
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+928.1026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1496
_reflns_number_gt                14922
_reflns_number_total             17547
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b209792c.txt
_cod_data_source_block           rh2
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7113905