Synthesis of a 1-aza-2-phospha-acenaphthene complex profiting from coordination enabled chloromethane elimination
Biskup, David; Bergmann, Tom; Schnakenburg, Gregor; Gomila, Rosa M.; Frontera, Antonio; Streubel, Rainer; RSC Advances 13 (2023) 21313–21317; doi:10.1039/D3RA04352E

data_7247045
_publ_section_title
;
 Synthesis of a 1-aza-2-phospha-acenaphthene complex profiting from
 coordination enabled chloromethane elimination
;
_journal_issue                   31
_journal_name_full               'RSC Advances'
_journal_page_first              21313
_journal_page_last               21317
_journal_paper_doi               10.1039/D3RA04352E
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C16 H10 N O6 P W'
_chemical_formula_sum            'C16 H10 N O6 P W'
_chemical_formula_weight         527.07
_chemical_name_systematic        TB037P.K
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-03-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-03-20 deposited with the CCDC.	2023-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.642(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1981(5)
_cell_length_b                   14.8394(12)
_cell_length_c                   13.0755(8)
_cell_measurement_reflns_used    3907
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.44
_cell_measurement_theta_min      2.65
_cell_volume                     1741.5(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.00
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
 110 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1460
_diffrn_reflns_av_unetI/netI     0.1049
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4632
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.244
_diffrn_reflns_theta_min         2.105
_exptl_absorpt_coefficient_mu    6.756
_exptl_absorpt_correction_T_max  0.3453
_exptl_absorpt_correction_T_min  0.1279
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.265
_refine_diff_density_min         -3.487
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         1587
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0768
_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^)+(0.1335P)^2^+2.9011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2165
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1254
_reflns_number_total             1587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra04352e2.cif
_cod_data_source_block           7
_cod_database_code               7247045
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.729
_shelx_estimated_absorpt_t_min   0.376
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: H1(0.5) N7(0.5) C1(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5) C6(0.5)
 H6(0.5) C7(0.5) C2(0.5) C3(0.5) C10(0.5) H10(0.5) C9(0.5) H9(0.5) C8(0.5)
 H8(0.5) C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C9(H9), C8(H8)
5.b Fitted hexagon refined as free rotating group:
 C7(C2,C3,C10,C9,C8)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              8945
_olex2_submission_special_instructions 'No special instructions were received'