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_7714316
_publ_section_title
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 Bicyclic (Alkyl)(Amino)Carbene (BICAAC) Supported Phosphinidenes
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02765A
_journal_year                    2023
_chemical_formula_moiety         'C22 H33 I N P'
_chemical_formula_sum            'C22 H33 I N P'
_chemical_formula_weight         469.36
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-05-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_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                   15.5985(9)
_cell_length_b                   19.4320(13)
_cell_length_c                   29.7451(16)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.030
_cell_measurement_theta_min      2.504
_cell_volume                     9016.0(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            81806
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         1.892
_exptl_absorpt_coefficient_mu    1.497
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0831 before and 0.0668 after correction.
The Ratio of minimum to maximum transmission is 0.8357.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         9211
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0455P)^2^+10.4224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5602
_reflns_number_total             9211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02765a2.cif
_cod_data_source_block           sk_ry_bicaacpiritu_0m_a
_cod_database_code               7714316
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.725
_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
 I1-P1 \\sim I1A-P1
 with sigma of 0.02
 I2-P2 \\sim I2A-P2
 with sigma of 0.02
3. Others
 Sof(I1A)=1-FVAR(1)
 Sof(I1)=FVAR(1)
 Sof(I2A)=1-FVAR(2)
 Sof(I2)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C40(H40), C43(H43), C20(H20), C17(H17), C7(H7), C25(H25)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C33(H33A,H33B), C28(H28A,H28B), C4(H4A,H4B), C3(H3A,H3B),
 C29(H29A,H29B)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C38(H38), C37(H37), C36(H36)
4.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C41(H41A,H41B,H41C), C8(H8A,H8B,H8C), C42(H42A,H42B,
 H42C), C45(H45A,H45B,H45C), C22(H22A,H22B,H22C), C44(H44A,H44B,H44C), C21(H21A,
 H21B,H21C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C),
 C32(H32A,H32B,H32C), C10(H10A,H10B,H10C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              28695
_olex2_submission_special_instructions 'No special instructions were received'