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_7238117
_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+, Br 1-, 1.5(H2 O2), 0.5(H2 O)'
_chemical_formula_sum            'C24 H24 Br O3.5 P'
_chemical_formula_weight         479.31
_chemical_name_systematic
;
Tetraphenylphosphonium bromide, hydrogenperoxide water solvate
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.889(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8495(6)
_cell_length_b                   16.3505(9)
_cell_length_c                   12.8342(7)
_cell_measurement_reflns_used    5578
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.25
_cell_volume                     2275.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1K'
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16101
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.901
_exptl_absorpt_correction_T_max  0.9109
_exptl_absorpt_correction_T_min  0.4499
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0470P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                3750
_reflns_number_total             5486
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b511834d.txt
_cod_data_source_block           2b
_cod_original_formula_sum        'C24 H24 Br O3.50 P'
_cod_database_code               7238117