Bicyclic (Alkyl)(Amino)Carbene (BICAAC) Supported Phosphinidenes
Kundu, Subrata; Yadav, Ritu; Das, Bindusagar; Singh, Ashi; Anmol, Anmol; Sharma, Ankita; Majumder, Chinmoy; Dalton Transactions  (2023) –; doi:10.1039/D3DT02765A

data_7714315
_publ_section_title
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 Bicyclic (Alkyl)(Amino)Carbene (BICAAC) Supported Phosphinidenes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02765A
_journal_year                    2023
_chemical_formula_moiety         '2(C22 H33 N P)'
_chemical_formula_sum            'C44 H66 N2 P2'
_chemical_formula_weight         684.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-05-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-23 deposited with the CCDC.	2023-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   24.690(3)
_cell_length_b                   35.674(4)
_cell_length_c                   18.131(2)
_cell_measurement_reflns_used    5713
_cell_measurement_temperature    109(2)
_cell_measurement_theta_max      0.989
_cell_measurement_theta_min      0.972
_cell_volume                     15970(3)
_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      109.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-IV CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39142
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.006
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Multi-scan
_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    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             5984
_exptl_crystal_preparation       'slow evaporation'
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 1994 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.43(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7829
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0703
_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^)+(0.0871P)^2^+46.6752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1942
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.914
_reflns_number_gt                5713
_reflns_number_total             7829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02765a2.cif
_cod_data_source_block           bicppritu_0ma_a
_cod_database_code               7714315
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.972
_olex2_refinement_description
;
1. Restrained distances
 C7-C10_2 \\sim C7A-C10_2
 with sigma of 0.02
 C7-C10_2 \\sim C7-C10A
 with sigma of 0.02
 C7A-C10_2 \\sim C7A-C10A
 with sigma of 0.02
 C4-C10_2 \\sim C4-C10A
 with sigma of 0.02
 C5-C10_2 \\sim C5-C10A
 with sigma of 0.02
 C8-C10_2 \\sim C8-C10A
 with sigma of 0.02
 C6-C10_2 \\sim C6-C10A
 with sigma of 0.02
 C10_2-C11_2 \\sim C10A-C11_2
 with sigma of 0.02
 C2_1-C10_1 \\sim C2_1-C20A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C10_2) = Uanis(C2_1)
3. Others
 Fixed Sof: H2AA(0.5) H2AB(0.5) H2BC(0.5) H2BD(0.5) H3BC(0.5) H3BD(0.5)
 H3AA(0.5) H3AB(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C7A(0.5) H7AA(0.5)
 H7AB(0.5) H7AC(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 C8(0.5) H8(0.5) C6(0.5) H6(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C10(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) C10A(0.5) C20A(0.4) H20A(0.4) H20B(0.4)
 H20C(0.4) C10(0.6) H10A(0.6) H10B(0.6) H10C(0.6) C10(0.5)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C6(H6), C7(H7), C20(H20), C17(H17), C12(H12), C14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD), C3(H3BC,H3BD), C3(H3AA,H3AB), C4(H4A,H4B),
 C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B), C3(H3A,H3B)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C3(H3), C4(H4), C5(H5)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C20A(H20A,H20B,H20C), C22(H22A,H22B,H22C), C19(H19A,H19B,
 H19C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C21(H21A,H21B,
 H21C), C18(H18A,H18B,H18C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              58097
_olex2_submission_special_instructions 'No special instructions were received'