The Room-Temperature Superstructure of ZrP2O7Is Orthorhombic: There Are No Unusual 180° P−O−P Bond Angles
Birkedal, Henrik; Krogh Andersen, Anne Marie; Arakcheeva, Alla; Chapuis, Gervais; Norby, Poul; Pattison, Philip; Inorganic Chemistry 45 (2006) 4346–4351; doi:10.1021/ic0600174

data_4332147
_publ_section_title
;
 The Room-Temperature Superstructure of ZrP2O7Is Orthorhombic:&#x00A0;
 There Are No Unusual 180\% P&#x2212;O&#x2212;P Bond Angles
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4346
_journal_page_last               4351
_journal_paper_doi               10.1021/ic0600174
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'O7 P2 Zr'
_chemical_formula_sum            'O7 P2 Zr'
_chemical_formula_weight         265.16
_chemical_name_common            'Zirconium pyrophosphate'
_chemical_name_systematic
; 
 Zirconium pyrophosphate 
;
_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_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            108
_cell_length_a                   24.7390(2)
_cell_length_b                   24.71841(19)
_cell_length_c                   24.7431(2)
_cell_measurement_temperature    293(2)
_cell_volume                     15130.6(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'synchrotron, BM-1 at ESRF'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1122
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            532466
_diffrn_reflns_theta_full        32.76
_diffrn_reflns_theta_max         32.76
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    2.511
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             13608
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.820
_refine_diff_density_min         -2.535
_refine_diff_density_rms         0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1222
_refine_ls_number_reflns         27901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1619
_reflns_number_gt                22764
_reflns_number_total             27901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0600174sup1.cif
_cod_data_source_block           all-nomerwght-renam
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4332147