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_7707271
_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 N3 P2 Si2'
_chemical_formula_sum            'C36 H45 N3 P2 Si2'
_chemical_formula_weight         637.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.056(2)
_cell_length_b                   16.625(3)
_cell_length_c                   15.563(2)
_cell_measurement_reflns_used    21114
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      1.897
_cell_volume                     3636.8(10)
_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      293
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker-APEX II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21114
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.930
_diffrn_reflns_theta_max         24.930
_diffrn_reflns_theta_min         1.897
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.124
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
;
 Flack x determined using 1268 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         3161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0281
_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^+0.5587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.782
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                2997
_reflns_number_total             3161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01091c2.cif
_cod_data_source_block           Ligand
_cod_depositor_comments
'Adding full bibliography for 7707271--7707274.cif.'
_cod_database_code               7707271
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.975
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
1.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
1.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C11(H11), C14(H14), C15(H15), C9(H9), C18(H18), C13(H13), C8(H8),
 C12(H12), C7(H7), C6(H6)
;
_shelx_res_checksum              95012
_shelx_hkl_checksum              94295
_olex2_submission_special_instructions 'No special instructions were received'