Novel primary phosphinecarboxamides derived from diamines.
Faria, Erica N.; Jupp, Andrew R.; Goicoechea, Jose M.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6991–6996; doi:10.1039/d1dt01198g

data_7707227
_publ_section_title
;
 Novel primary phosphinecarboxamides derived from diamines.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6991
_journal_page_last               6996
_journal_paper_doi               10.1039/d1dt01198g
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C H5 N2 O P'
_chemical_formula_sum            'C H5 N2 O P'
_chemical_formula_weight         92.04
_chemical_name_systematic
;
 PH2C(O)NHNH2
;
_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'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-04-12 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.901(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.025(2)
_cell_length_b                   4.8946(4)
_cell_length_c                   6.9706(10)
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_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.0820
_cell_measurement_theta_min      7.0990
_cell_volume                     851.83(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5153
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.470
_diffrn_reflns_theta_max         66.470
_diffrn_reflns_theta_min         3.540
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       needle
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1500
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0788
_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^)+(0.0798P)^2^+4.9532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1033
_reflns_number_total             1500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01198g2.cif
_cod_data_source_block           EF184
_cod_depositor_comments
'Adding full bibliography for 7707227--7707230.cif.'
_cod_original_cell_volume        851.85(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7707227
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.509
_shelx_estimated_absorpt_t_max   0.918
_shelx_res_checksum              1351