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_7220399
_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         'C11 H16 O4 P, C2 H8 N'
_chemical_formula_sum            'C13 H24 N O4 P'
_chemical_formula_weight         289.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 111.738(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.989(5)
_cell_length_b                   9.027(4)
_cell_length_c                   14.006(5)
_cell_measurement_reflns_used    5267
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1
_cell_measurement_theta_min      2.9
_cell_volume                     1525.4(10)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
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_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
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_diffrn_ambient_temperature      100(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  0.0388
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9896
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.818
_diffrn_source                   'Sealed Tube'
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_exptl_absorpt_correction_T_max  1.000
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            colorless
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_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.210
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_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0313P)^2^+1.1205P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2620
_reflns_number_total             2836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00675a2.cif
_cod_data_source_block           ALP-HYDRO-PHOS-DMF
_cod_depositor_comments
'Adding full bibliography for 7220395--7220401.cif.'
_cod_database_code               7220399
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2012-9
_shelx_res_checksum              18770