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_7059111
_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         '2(C16 H21 Cu I N5)'
_chemical_formula_sum            'C32 H42 Cu2 I2 N10'
_chemical_formula_weight         947.63
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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            8
_cell_length_a                   18.092(5)
_cell_length_b                   18.092(5)
_cell_length_c                   21.761(8)
_cell_measurement_reflns_used    83160
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.997
_cell_measurement_theta_min      1.126
_cell_volume                     7123(4)
_computing_data_collection       apex2
_computing_molecular_graphics    ortep
_computing_publication_material  CIFTAB
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            83078
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.464
_exptl_absorpt_coefficient_mu    2.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       Block
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   1
_exptl_transmission_factor_min   0.78
_refine_diff_density_max         1.929
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6283
_refine_ls_number_restraints     387
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0504
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.750
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4507
_reflns_number_total             6283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01009e2.cif
_cod_data_source_block           cu2I2
_cod_database_code               7059111
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.617
_shelx_estimated_absorpt_t_min   0.573
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50(6)
 0.50(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H38A,H38B,H38C} of C38, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  {H25A,H25B,H25C} of C25, {H60A,H60B,H60C} of C60, {H64A,H64B,H64C} of C64,
  {H66A,H66B,H66C} of C66, {H77A,H77B,H77C} of C77, {H30A,H30B,H30C} of C30,
  {H22A,H22B,H22C} of C22
3. Rigid body (RIGU) restrains
 C23, I10, Cu11, Cu12, N13, N14, N15, C16, N17, C18, C19, C20, C21, C22, C24,
 C25, C26, C29, C30, C37, C38, N43, C44, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cu50, I51, N52, N53, N54, C55, N56, C57, C58, C59, C60, C61, C62, C63, C64,
 C65, C66, C67, C76, C77, N85, C86, N87, C88
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C62(H62A,H62B), C19(H19A,H19B), C59(H59A,H59B)
4.b Aromatic/amide H refined with riding coordinates:
 N85(H85), N43(H43), N87(H87), C44(H44), C61(H61), C21(H21), C65(H65),
 C26(H26), C86(H86), C88(H88), C48(H48)
4.c Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C77(H77A,H77B,H77C), C30(H30A,H30B,H30C), C64(H64A,H64B,
 H64C), C25(H25A,H25B,H25C), C60(H60A,H60B,H60C), C38(H38A,H38B,H38C), C22(H22A,
 H22B,H22C)
;
_shelx_res_checksum              74366
_olex2_submission_special_instructions 'No special instructions were received'