From Coordinated Oxophosphinidene to O,O,P-Bound Arylhypophosphite(2-) To Build a Singular Mo2Sn2O4P2 Metallocycle
María Alonso; M. Angeles Alvarez; M. Esther García; Miguel A. Ruiz; Inorganic Chemistry 47 (2008) 1252–1254; doi:10.1021/ic702416z

data_4304837
_publ_section_title
;
From Coordinated Oxophosphinidene to O,O,P-Bound Arylhypophosphite(2-) To
Build a Singular Mo2Sn2O4P2 Metallocycle
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1252
_journal_page_last               1254
_journal_paper_doi               10.1021/ic702416z
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C62 H82 Mo2 O10 P2 Sn2, 2(C4 H8 O)'
_chemical_formula_sum            'C70 H98 Mo2 O12 P2 Sn2'
_chemical_formula_weight         1622.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-05-24T12:49:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.748(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.449(7)
_cell_length_b                   14.367(5)
_cell_length_c                   27.400(10)
_cell_measurement_reflns_used    1157
_cell_measurement_temperature    120.0(1)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.355
_cell_measurement_wavelength     0.71073
_cell_volume                     7496(5)
_computing_cell_refinement       'Brucker Smart'
_computing_data_collection       'Brucker Smart'
_computing_data_reduction        'Brucker Smart'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (1999)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30737
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.863
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         7696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                5263
_reflns_number_total             7696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702416z-file002_1.cif
_cod_data_source_block           compound4-2Tol
_cod_database_code               4304837