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_7040287
_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 H50 N4 O2, 0.5(C4 O2)'
_chemical_formula_sum            'C44 H50 N4 O3'
_chemical_formula_weight         682.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 94.704(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2424(2)
_cell_length_b                   22.8992(7)
_cell_length_c                   27.3834(8)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      21.716
_cell_measurement_theta_min      2.322
_cell_volume                     3901.2(2)
_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 0.9998
_diffrn_measured_fraction_theta_max 0.9998
_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  0.0492
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            75008
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         1.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.7054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0909 before and 0.0519 after correction.
The Ratio of minimum to maximum transmission is 0.9468.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.1626
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464.6099
_exptl_crystal_recrystallization_method 'slow evaporation of ethyl acetate'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.3549
_refine_diff_density_min         -0.2768
_refine_diff_density_rms         0.0597
_refine_ls_d_res_high            0.8700
_refine_ls_d_res_low             13.6456
_refine_ls_goodness_of_fit_ref   1.0674
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    89
_refine_ls_number_parameters     519
_refine_ls_number_reflns         6196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0674
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+1.4377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -7
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              -5
_reflns_number_gt                4586
_reflns_number_total             6196
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt02389d2.cif
_cod_data_source_block           hardy012815
_cod_depositor_comments
'Adding full bibliography for 7040285--7040288.cif.'
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_database_code               7040287
_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, All O(H) groups
2. Rigid bond restraints
 C1A, C1b, C2A, C2b, C3A, C3b
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Same fragment restrains
{C1A, C1b, C2A, C2b, C3A, C3b} sigma for 1-2: 0.02, 1-3: 0.04
as
{C1AA, N1, O1, C2AA, N2, O2}
4. Others
 Sof(C1b)=Sof(C2b)=Sof(C3b)=Sof(H1ba)=Sof(H1bb)=Sof(H1bc)=Sof(H2ba)=Sof(H2bb)=
 Sof(H2bc)=Sof(H3ba)=Sof(H3bb)=Sof(H3bc)=1-FVAR(1)
 Sof(C1A)=Sof(C2A)=Sof(C3A)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=Sof(H2Aa)=Sof(H2Ab)=
 Sof(H2Ac)=Sof(H3Aa)=Sof(H3Ab)=Sof(H3Ac)=FVAR(1)
 Fixed Sof: C44S(0.5) C45S(0.5) O46S(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C15(H15), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23),
 C26(H26), C28(H28), C30(H30), C36(H36)
5.b Idealised Me refined as rotating group:
 C6AA(H6Aa,H6Ab,H6Ac), C5(H5a,H5b,H5c), C9AA(H9Aa,H9Ab,H9Ac), C33(H33a,H33b,
 H33c), C34(H34a,H34b,H34c), C35(H35a,H35b,H35c), C39(H39a,H39b,H39c), C40(H40a,
 H40b,H40c), C41(H41a,H41b,H41c), C1A(H1Aa,H1Ab,H1Ac), C2A(H2Aa,H2Ab,H2Ac),
 C3A(H3Aa,H3Ab,H3Ac), C1b(H1ba,H1bb,H1bc), C2b(H2ba,H2bb,H2bc), C3b(H3ba,H3bb,
 H3bc)
5.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_olex2_exptl_crystal_mounting_method 'mounted on a glass fibre in paratone oil'
_olex2_submission_special_instructions 'No special instructions were received'