2,6-Dimethylphenol derived H-phosphonate and α-hydroxyphosphonate: facile synthesis, crystal chemistry, supramolecular association and metal complexation
Hossain, Sazzat; Gupta, Sandeep K.; Murugavel, Ramaswamy; CrystEngComm 17 (2015) 4355–; doi:10.1039/C5CE00675A

data_7220395
_publ_section_title
;
 2,6-Dimethylphenol derived H-phosphonate and \a-hydroxyphosphonate:
 facile synthesis, crystal chemistry, supramolecular association and metal
 complexation
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              4355
_journal_paper_doi               10.1039/C5CE00675A
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C8 H11 O3 P'
_chemical_formula_sum            'C8 H11 O3 P'
_chemical_formula_weight         186.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_audit_update_record
;
2015-04-03 deposited with the CCDC.
2015-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.265(5)
_cell_length_b                   7.246(2)
_cell_length_c                   8.860(3)
_cell_measurement_reflns_used    1960
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.20
_cell_measurement_theta_min      2.70
_cell_volume                     915.8(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6730
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.495
_diffrn_reflns_theta_min         2.811
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.146
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 640 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.15(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1582
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+0.3627P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.732
_reflns_Friedel_fraction_full    0.845
_reflns_Friedel_fraction_max     0.843
_reflns_number_gt                1568
_reflns_number_total             1582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00675a2.cif
_cod_data_source_block           HY-PHOS
_cod_depositor_comments
'Adding full bibliography for 7220395--7220401.cif.'
_cod_database_code               7220395
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.949
_shelxl_version_number           2012-9
_shelx_res_checksum              49640