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_7040288
_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         'C42 H48 N4 O3 V'
_chemical_formula_sum            'C42 H48 N4 O3 V'
_chemical_formula_weight         707.82
_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             2016-07-15
_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                77.715(1)
_cell_angle_beta                 74.447(1)
_cell_angle_gamma                79.226(1)
_cell_formula_units_Z            2
_cell_length_a                   10.5213(4)
_cell_length_b                   12.7581(5)
_cell_length_c                   16.9448(6)
_cell_measurement_reflns_used    6818
_cell_measurement_temperature    296
_cell_measurement_theta_max      25.142
_cell_measurement_theta_min      2.25
_cell_volume                     2120.59(14)
_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      296.15
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9999
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35450
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0747 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.9119.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.1084
_exptl_crystal_description       prism
_exptl_crystal_F_000             750.9234
_exptl_crystal_recrystallization_method
'slow diffusion of methanol into a concentrated THF solution'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.3246
_refine_diff_density_min         -0.3191
_refine_diff_density_rms         0.0743
_refine_ls_d_res_high            0.8500
_refine_ls_d_res_low             12.3467
_refine_ls_goodness_of_fit_ref   1.0591
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    72
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0591
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0660P)^2^+1.7481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                5678
_reflns_number_total             7239
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt02389d2.cif
_cod_data_source_block           bam150_0m
_cod_depositor_comments
'Adding full bibliography for 7040285--7040288.cif.'
_cod_database_code               7040288
_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.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C26(H26), C17(H17), C23(H23), C20(H20), C22(H22), C21(H21),
 C30(H30), C28(H28), C15(H15), C36(H36)
2.b Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C4(H4a,H4b,H4c), C6(H6a,H6b,H6c), C11(H11a,H11b,H11c),
 C10(H10a,H10b,H10c), C12(H12a,H12b,H12c), C34(H34a,H34b,H34c), C33(H33a,H33b,
 H33c), C41(H41a,H41b,H41c), C40(H40a,H40b,H40c), C39(H39a,H39b,H39c), C35(H35a,
 H35b,H35c)
;
_olex2_submission_special_instructions 'No special instructions were received'