Synthesis, structural characterization, and bonding analysis of two-coordinate copper(I) and silver(I) complexes of pyrrole-based bis(phosphinimine): new metal-pyrrole ring π-interactions.
Jha, Vikesh Kumar; Das, Sanghamitra; Subramaniyan, Vasudevan; Guchhait, Tapas; Dakua, Kishan Kumar; Mishra, Sabyashachi; Mani, Ganesan; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8036–8044; doi:10.1039/d1dt01091c

data_7707272
_publ_section_title
;
 Synthesis, structural characterization, and bonding analysis of
 two-coordinate copper(I) and silver(I) complexes of pyrrole-based
 bis(phosphinimine): new metal-pyrrole ring \p-interactions.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8036
_journal_page_last               8044
_journal_paper_doi               10.1039/d1dt01091c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C36 H45 Cu N3 P2 Si2, Cl2 Cu'
_chemical_formula_sum            'C36 H45 Cl2 Cu2 N3 P2 Si2'
_chemical_formula_weight         835.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-17
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-31 deposited with the CCDC.	2021-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                63.551(2)
_cell_angle_beta                 76.619(2)
_cell_angle_gamma                83.611(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3861(10)
_cell_length_b                   12.8347(11)
_cell_length_c                   13.8430(12)
_cell_measurement_reflns_used    22589
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1.5
_cell_volume                     1916.7(3)
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker-APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22589
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.945
_diffrn_reflns_theta_max         24.945
_diffrn_reflns_theta_min         1.678
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.114
_refine_diff_density_max         1.580
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         6647
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0617P)^2^+2.9746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5586
_reflns_number_total             6647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01091c2.cif
_cod_data_source_block           Cu_CuCl2
_cod_depositor_comments
'Adding full bibliography for 7707271--7707274.cif.'
_cod_database_code               7707272
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.674
_olex2_refinement_description
;
1. Restrained distances
 N3-Si2A \\sim N3-Si2B
 with sigma of 0.02
 C35A-Si2A \\sim C35B-Si2B
 with sigma of 0.02
 Si2A-C34A \\sim Si2B-C34B
 with sigma of 0.02
 Si2A-C36A \\sim Si2B-C36B
 with sigma of 0.02
 C34A-C36A \\sim C34B-C36B
 with sigma of 0.04
 N3-C35A \\sim N3-C35B
 with sigma of 0.04
 N3-C34A \\sim N3-C34B
 with sigma of 0.04
 N3-C36A \\sim N3-C36B
 with sigma of 0.04
 C35A-C34A \\sim C35B-C34B
 with sigma of 0.04
 C35A-C36A \\sim C35B-C36B
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
Uanis(C35A) = Uanis(C35B) = Uanis(Si2A) = Uanis(Si2B) = Uanis(C36B) =
Uanis(C36A) = Uanis(C34B) = Uanis(C34A)
3. Rigid body (RIGU) restrains
 Si2B, Si2A, C35A, C35B, C34A, C34B, C36A, C36B, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(Si2B)=Sof(C34B)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(Si2A)=Sof(C34A)=Sof(H34A)=
 Sof(H34B)=Sof(H34C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C21(H21A,H21B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C35A(H35A,H35B,H35C),
 C34A(H34A,H34B,H34C), C36A(H36A,H36B,H36C), C35B(H35D,H35E,H35F), C34B(H34D,
 H34E,H34F), C36B(H36D,H36E,H36F)
;
_shelx_res_checksum              2757
_shelx_hkl_checksum              97004
_olex2_submission_special_instructions 'No special instructions were received'