Non-Interpenetrating Transition Metal Diorganophosphate 2-Dimensional Rectangular Grids from Their 1-Dimensional Wires: Structural Transformations under Mild Conditions
Ramasamy Pothiraja; Malaichamy Sathiyendiran; Ray J. Butcher; Ramaswamy Murugavel; Inorganic Chemistry 44 (2005) 6314–6323; doi:10.1021/ic050742z

data_4309540
_publ_section_title
;
Non-Interpenetrating Transition Metal Diorganophosphate 2-Dimensional
Rectangular Grids from Their 1-Dimensional Wires: Structural
Transformations under Mild Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6314
_journal_page_last               6323
_journal_paper_doi               10.1021/ic050742z
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C10 H14 N2 O8 P2'
_chemical_formula_weight         352.17
_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                 98.55(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.67400(10)
_cell_length_b                   18.036(8)
_cell_length_c                   8.161(2)
_cell_measurement_temperature    133(2)
_cell_volume                     680.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6793
_diffrn_reflns_theta_full        24.67
_diffrn_reflns_theta_max         24.67
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.365
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0306P)^2^+0.4738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                1079
_reflns_number_total             1157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050742zsi20050511_053247_5.cif
_cod_data_source_block           mur60(Compound7,Organic_phosphate)
_cod_original_cell_volume        680.4(4)
_cod_database_code               4309540