Synthesis, Spectroscopic Study and Crystal Structure of a New Amidophosphonate, (C<sub>6</sub>H<sub>5</sub>O)<sub>2</sub>P(O)(NHCH(CH<sub>3</sub>)(C<sub>2</sub>H<sub>5</sub>))
HAMZEHEE, Farahnaz; POURAYOUBI, Mehrdad; CHOQUESILLO-LAZARTE, Duane; X-ray Structure Analysis Online 32 (2016) 47–; doi:10.2116/xraystruct.32.47

data_1551610
_publ_section_title
;
 Synthesis, Spectroscopic Study and Crystal Structure of a New
 Amidophosphonate,
 (C&lt;sub&gt;6&lt;/sub&gt;H&lt;sub&gt;5&lt;/sub&gt;O)&lt;sub&gt;2&lt;/sub&gt;P(O)(NHCH(CH&lt;sub&gt;3&lt;/sub&gt;)(C&lt;sub&gt;2&lt;/sub&gt;H&lt;sub&gt;5&lt;/sub&gt;))
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              47
_journal_paper_doi               10.2116/xraystruct.32.47
_journal_volume                  32
_journal_year                    2016
_chemical_formula_moiety         'C16 H20 N O3 P'
_chemical_formula_sum            'C16 H20 N O3 P'
_chemical_formula_weight         305.30
_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_date             2016-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.542(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.277(2)
_cell_length_b                   5.2887(7)
_cell_length_c                   21.962(5)
_cell_measurement_reflns_used    635
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.89
_cell_measurement_theta_min      3.36
_cell_volume                     1520.8(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2661
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.045
_diffrn_reflns_theta_max         25.045
_diffrn_reflns_theta_min         2.233
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.745159
_exptl_absorpt_correction_T_min  0.642897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0822 before and 0.0425 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0869 before and 0.0492 after correction.
 The Ratio of minimum to maximum transmission is 0.86.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 11947 reflections, Rint = 0.0874
 (4186 with I > 3sig(I), Rint = 0.0424)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2661
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0725
_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^)+(0.0606P)^2^+3.8008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1995
_reflns_number_total             2661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            32_47_1.txt
_cod_data_source_block           fh25
_cod_database_code               1551610
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.712(3) 0.288(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 C2, C1, C3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Riding coordinates:
 N1(H1)
4.b Ternary CH refined with riding coordinates:
 C1(H1A)
4.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
4.d Aromatic/amide H refined with riding coordinates:
 C16(H16), C7(H7), C10(H10), C6(H6), C12(H12), C15(H15), C14(H14), C9(H9),
 C8(H8), C13(H13)
4.e Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              56425
_shelx_hkl_checksum              68244
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'