Synthesis, Characterization, and Crystal Structures of Two Divalent Metal Diphosphonates with a Layered and a 3D Network Structure
Jiang-Gao Mao; Zhike Wang; Abraham Clearfield; Inorganic Chemistry 41 (2002) 2334–2340; doi:10.1021/ic011202e

data_4317945
_publ_section_title
;
 Synthesis, Characterization, and Crystal Structures of Two Divalent Metal
 Diphosphonates with a Layered and a 3D Network Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2334
_journal_page_last               2340
_journal_paper_doi               10.1021/ic011202e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C6 H24 Mn N2 O14 P4'
_chemical_formula_weight         527.09
_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                82.009(6)
_cell_angle_beta                 74.356(6)
_cell_angle_gamma                89.853(6)
_cell_formula_units_Z            2
_cell_length_a                   9.224(3)
_cell_length_b                   9.780(3)
_cell_length_c                   10.554(3)
_cell_measurement_temperature    293(2)
_cell_volume                     907.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       'narrow frame methods'
_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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5307
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.10
_diffrn_standards_interval_time  <1.0%
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            light_pink
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1084P)^2^+4.4030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.2158
_reflns_number_gt                2161
_reflns_number_total             3681
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic011202e_1.cif
_cod_data_source_block           maoc9
_cod_original_cell_volume        907.4(5)
_cod_database_code               4317945