The preparation and crystal structures of novel perhydrates Ph4X+Hal‒·nH2O2: anionic hydrogen-bonded chains containing hydrogen peroxide
Churakov, Andrei V.; Prikhodchenko, Petr V.; Howard, Judith A. K.; CrystEngComm 7 (2005) 664–; doi:10.1039/b511834d

data_7238115
_publ_section_title
;
 The preparation and crystal structures of novel perhydrates
 Ph4X+Hal--&#x00B7;nH2O2: anionic hydrogen-bonded chains containing
 hydrogen peroxide
;
_journal_issue                   110
_journal_name_full               CrystEngComm
_journal_page_first              664
_journal_paper_doi               10.1039/b511834d
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety
'C24 H20 P 1+, Cl 1-, 1.73(H2 O2), 0.27(H2 O)'
_chemical_formula_sum            'C24 H24 Cl O3.73 P'
_chemical_formula_weight         438.53
_chemical_name_systematic
;
Tetraphenylphosphonium chloride, hydrogenperoxide water solvate
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.131(1)
_cell_angle_beta                 73.415(1)
_cell_angle_gamma                71.343(1)
_cell_formula_units_Z            2
_cell_length_a                   9.6029(6)
_cell_length_b                   11.1280(7)
_cell_length_c                   11.5333(7)
_cell_measurement_reflns_used    3800
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.99
_cell_measurement_theta_min      2.64
_cell_volume                     1100.42(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       \w
_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  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8476
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.9602
_exptl_absorpt_correction_T_min  0.9350
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0487P)^2^+0.5612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                4477
_reflns_number_total             5069
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b511834d.txt
_cod_data_source_block           1b
_cod_database_code               7238115