Pillared Layered Structures Based upon M(III) Ethylene Diphosphonates: The Synthesis and Crystal Structures of MIII(H2O)(HO3P(CH2)2PO3) (M = Fe, Al, Ga)
Crystal A. Merrill; Anthony K. Cheetham; Inorganic Chemistry 44 (2005) 5273–5277; doi:10.1021/ic0502269

data_4309264
_publ_section_title
;
Pillared Layered Structures Based upon M(III) Ethylene Diphosphonates:
The Synthesis and Crystal Structures of MIII(H2O)(HO3P(CH2)2PO3) (M = Fe,
Al, Ga)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5273
_journal_page_last               5277
_journal_paper_doi               10.1021/ic0502269
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C2 H2 Fe O7 P2'
_chemical_formula_weight         255.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.739(5)
_cell_length_b                   9.498(5)
_cell_length_c                   15.940(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1474.5(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_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  0.0877
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8286
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    2.475
_exptl_crystal_density_diffrn    2.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1617
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0568P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                1181
_reflns_number_total             1617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0502269si20050215_055443.cif
_cod_data_source_block           cmi164m
_cod_original_cell_volume        1474.4(13)
_cod_database_code               4309264