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_7714317
_publ_section_title
;
 Bicyclic (Alkyl)(Amino)Carbene (BICAAC) Supported Phosphinidenes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02765A
_journal_year                    2023
_chemical_formula_moiety         'C22 H33 Br N P'
_chemical_formula_sum            'C22 H33 Br N P'
_chemical_formula_weight         422.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-05-10
_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            8
_cell_length_a                   9.2049(8)
_cell_length_b                   16.6408(13)
_cell_length_c                   29.176(3)
_cell_measurement_reflns_used    3511
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      26.438
_cell_measurement_theta_min      2.448
_cell_volume                     4469.1(7)
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      302.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'BRUKER APEX IV'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            120954
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.438
_diffrn_reflns_theta_min         2.448
_exptl_absorpt_coefficient_mu    1.916
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4589
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+2.4723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3383
_reflns_number_total             4589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02765a2.cif
_cod_data_source_block           sk_ry_bicaacpbr_0m_a
_cod_database_code               7714317
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Br2-P1 \\sim Br1-P1
 with sigma of 0.02
3. Others
 Sof(Br1)=1-FVAR(1)
 Sof(Br2)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C17(H17), C20(H20)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15)
4.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C8(H8A,H8B,
 H8C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              85827
_olex2_submission_special_instructions 'No special instructions were received'