Solid state π-π stacking and higher order dimensional crystal packing, reactivity, and electrochemical behaviour of salphenazine actinide and transition metal complexes.
Hardy, E. E.; Eddy, M. A.; Maynard, B. A.; Gorden, A. E. V.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14243–14251; doi:10.1039/c6dt02389d

data_7040286
_publ_section_title
;
 Solid state \p-\p stacking and higher order dimensional crystal packing,
 reactivity, and electrochemical behaviour of salphenazine actinide and
 transition metal complexes.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14243
_journal_page_last               14251
_journal_paper_doi               10.1039/c6dt02389d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C43 H52 N4 O3 Zn'
_chemical_formula_sum            'C43 H52 N4 O3 Zn'
_chemical_formula_weight         738.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-15 deposited with the CCDC.
2016-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                105.875(2)
_cell_angle_beta                 100.257(2)
_cell_angle_gamma                91.511(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3102(5)
_cell_length_b                   15.1537(7)
_cell_length_c                   16.4769(8)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      27.87
_cell_measurement_theta_min      2.17
_cell_volume                     2193.30(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.45
_diffrn_measured_fraction_theta_full 0.9951
_diffrn_measured_fraction_theta_max 0.9951
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43775
_diffrn_reflns_theta_full        25.7232
_diffrn_reflns_theta_max         25.72
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1335 before and 0.0677 after correction. The Ratio of minimum to maximum transmission is 0.8503. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.1179
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             784.9006
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/THF'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.5904
_refine_diff_density_min         -0.6054
_refine_diff_density_rms         0.0903
_refine_ls_d_res_high            0.8188
_refine_ls_d_res_low             12.5314
_refine_ls_goodness_of_fit_ref   1.0636
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    76
_refine_ls_number_parameters     476
_refine_ls_number_reflns         8341
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0635
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+1.6034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1186
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              17
_reflns_limit_k_min              -18
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                6824
_reflns_number_total             8341
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt02389d2.cif
_cod_data_source_block           Emily05222015_0m
_cod_depositor_comments
'Adding full bibliography for 7040285--7040288.cif.'
_cod_database_code               7040286
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H3-O3
 0.94 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C3(H3a), C5(H5), C28(H28), C30(H30), C32(H32), C26(H26), C17(H17),
 C20(H20), C21(H21), C22(H22), C23(H23)
3.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C8(H8a,H8b,
 H8c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c), C37(H37a,H37b,H37c), C38(H38a,H38b,
 H38c), C36(H36a,H36b,H36c), C42(H42a,H42b,H42c), C41(H41a,H41b,H41c), C40(H40a,
 H40b,H40c), C43(H43a,H43b,H43c)
;
_olex2_submission_special_instructions 'No special instructions were received'