Di-tert-butyl Phosphate as Synthon for Metal Phosphate Materials via Single-Source Coordination Polymers [M(dtbp)2]n (M = Mn, Cu) and [Cd(dtbp)2(H2O)]n (dtbp-H = (tBuO)2P(O)OH)
Malaichamy Sathiyendiran; Ramaswamy Murugavel; Inorganic Chemistry 41 (2002) 6404–6411; doi:10.1021/ic0259787

data_4318976
_publ_section_title
;
 Di-tert-butyl Phosphate as Synthon for Metal Phosphate Materials via
 Single-Source Coordination Polymers [M(dtbp)2]n (M = Mn, Cu) and
 [Cd(dtbp)2(H2O)]n (dtbp-H = (tBuO)2P(O)OH)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6404
_journal_page_last               6411
_journal_paper_doi               10.1021/ic0259787
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C48 H114 Cd3 O27 P6'
_chemical_formula_weight         1646.4
_chemical_name_systematic
;
 ?
;
_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                84.54(3)
_cell_angle_beta                 79.43(3)
_cell_angle_gamma                70.03(3)
_cell_formula_units_Z            2
_cell_length_a                   12.689(3)
_cell_length_b                   14.364(3)
_cell_length_c                   22.491(5)
_cell_measurement_temperature    203(2)
_cell_volume                     3785.1(17)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        XPREP
_computing_molecular_graphics    Platon
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0111
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            9802
_diffrn_reflns_theta_full        22.54
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.030
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         9801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0205P)^2^+18.8200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                8268
_reflns_number_total             9801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0259787_s1_3.cif
_cod_data_source_block           mur19x(Compound3)
_cod_original_cell_volume        3784.9(13)
_cod_database_code               4318976