New types of Cu and Ag clusters supported by the pyrrole-based NNN-pincer type ligand
Jana, Oishi; Mani, Ganesan; New Journal of Chemistry 41 (2017) 9361–; doi:10.1039/C7NJ01009E

data_7059109
_publ_section_title
;
 New types of Cu and Ag clusters supported by the pyrrole-based NNN-pincer
 type ligand
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9361
_journal_paper_doi               10.1039/C7NJ01009E
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C32 H40 Cu N10'
_chemical_formula_sum            'C32 H40 Cu N10'
_chemical_formula_weight         628.28
_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             2017-05-09
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.03.14 svn.r3397 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2017-07-12 deposited with the CCDC.
2017-08-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   22.391(5)
_cell_length_b                   34.918(8)
_cell_length_c                   16.505(4)
_cell_measurement_reflns_used    25651
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.997
_cell_measurement_theta_min      2.959
_cell_volume                     12904(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    sir92
_diffrn_ambient_temperature      298.03
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-APEX-II CCD area detector'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25651
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.959
_exptl_absorpt_coefficient_mu    0.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       Block
_exptl_crystal_F_000             5296
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.7457
_exptl_transmission_factor_min   0.5271
_refine_diff_density_max         0.128
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         4717
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0345P)^2^+3.2654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4035
_reflns_number_total             4717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01009e2.cif
_cod_data_source_block           cunnn
_cod_original_cell_volume        12904(6)
_cod_database_code               7059109
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.865
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(3)
 0.45(3)
2. 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
3. Rigid body (RIGU) restrains
 C1, H1A, H1B, H1C, C2, C3, H3, C4, C5, H5A, H5B, H5C, C6, H6A, H6B, C7, C8,
 H8, C9, H9, C10, C11, H11A, H11B, C12, C13, H13A, H13B, H13C, C14, H14, C15,
 C16, H16A, H16B, H16C, N1, N2, N3B, N4, N5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, H1AA, H1AB, H1AC, C2A, C3A, H3A, N1A, C4A, N2A, C5A, H5AA, H5AB, H5AC,
 C6A, H6AA, H6AB, N5A, C7A, C10A, C15A, N4A, C8A, H8A, C9A, H9A, C11A, H11C,
 H11D, C14A, H14A, C16A, H16D, H16E, H16F, C12A, C13A, H13D, H13E, H13F, N3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) C3(0.5) H3(0.5) C4(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) C8(0.5)
 H8(0.5) C9(0.5) H9(0.5) C10(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5)
 C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5) H14(0.5) C15(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) H16C(0.5) N1(0.5) N2(0.5) N3B(0.5) N4(0.5) N5(0.5)
 C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C2A(0.5) C3A(0.5) H3A(0.5) N1A(0.5)
 C4A(0.5) N2A(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) H5AC(0.5) C6A(0.5) H6AA(0.5)
 H6AB(0.5) N5A(0.5) C7A(0.5) C10A(0.5) C15A(0.5) N4A(0.5) C8A(0.5) H8A(0.5)
 C9A(0.5) H9A(0.5) C11A(0.5) H11C(0.5) H11D(0.5) C14A(0.5) H14A(0.5) C16A(0.5)
 H16D(0.5) H16E(0.5) H16F(0.5) C12A(0.5) C13A(0.5) H13D(0.5) H13E(0.5)
 H13F(0.5) N3A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C11(H11A,H11B), C22(H22A,H22B), C27(H27A,H27B), C6A(H6AA,H6AB),
 C11A(H11C,H11D)
5.b Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C14(H14), C19(H19), C24(H24), C25(H25), C30(H30),
 C3A(H3A), C8A(H8A), C9A(H9A), C14A(H14A)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C),
 C1A(H1AA,H1AB,H1AC), C5A(H5AA,H5AB,H5AC), C16A(H16D,H16E,H16F), C13A(H13D,H13E,
 H13F)
;
_shelx_res_checksum              59289
_olex2_submission_special_instructions 'No special instructions were received'