Meridional vs. facial coordination geometries of a dipodal ligand framework featuring a secondary coordination sphere.
Matson, Ellen M.; Gordon, Zachary; Lin, Benjamin; Nilges, Mark J.; Fout, Alison R.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 16992–16995; doi:10.1039/c4dt02327g

data_7032823
_publ_section_title
;
 Meridional vs. facial coordination geometries of a dipodal ligand
 framework featuring a secondary coordination sphere.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16992
_journal_page_last               16995
_journal_paper_doi               10.1039/c4dt02327g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C25 H37 Cl2 Cu N5'
_chemical_formula_sum            'C25 H37 Cl2 Cu N5'
_chemical_formula_weight         542.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2918 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.85
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6057(4)
_cell_length_b                   16.4209(4)
_cell_length_c                   10.7318(3)
_cell_measurement_temperature    173(2)
_cell_volume                     2570.72(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.935
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19715
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.745
_diffrn_reflns_theta_min         1.396
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  0.8437
_exptl_absorpt_correction_T_min  0.6481
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         5660
_refine_ls_number_restraints     1157
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0500P)^2^+0.6980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1202
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3796
_reflns_number_total             5660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02327g2.cif
_cod_data_source_block           cm78eascopy
_cod_depositor_comments
'Adding full bibliography for 7032823--7032828.cif.'
_cod_database_code               7032823
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.844
_shelx_estimated_absorpt_t_min   0.648
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5-C20 \\sim N5-C20B
 with sigma of 0.01
 N1-C1 \\sim N1-C1B
 with sigma of 0.01
 N1-C2 \\sim N1-C2B \\sim N1-C14 \\sim N1-C14B
 with sigma of 0.01
 C14-C15 \\sim C14B-C15
 with sigma of 0.01
 C5-C6 \\sim C5B-C6
 with sigma of 0.01
 C6-C7 \\sim C6-C7B \\sim C6-C7C
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C20B \\sim C21B
\\sim C22B \\sim C23B \\sim C24B \\sim C25B: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C1 \\sim C14 \\sim C2 \\sim C3 \\sim N2 \\sim C4 \\sim C5 \\sim C1B \\sim C14B
\\sim C2B \\sim C3B \\sim N2B \\sim C4B \\sim C5B: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
C7 \\sim N3 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C7B
\\sim N3B \\sim C8B \\sim C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13B \\sim
C7C \\sim N3C \\sim C8C \\sim C9C \\sim C10C \\sim C11C \\sim C12C \\sim C13C:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C1B)
\\sim Ueq, Uanis(C14B) \\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(C3B) \\sim Ueq,
Uanis(N2B) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C5B) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C7B) \\sim Ueq, Uanis(N3B) \\sim Ueq, Uanis(C8B)
\\sim Ueq, Uanis(C9B) \\sim Ueq, Uanis(C10B) \\sim Ueq, Uanis(C11B) \\sim Ueq,
Uanis(C12B) \\sim Ueq, Uanis(C13B) \\sim Ueq, Uanis(C7C) \\sim Ueq, Uanis(N3C)
\\sim Ueq, Uanis(C8C) \\sim Ueq, Uanis(C9C) \\sim Ueq, Uanis(C10C) \\sim Ueq,
Uanis(C11C) \\sim Ueq, Uanis(C12C) \\sim Ueq, Uanis(C13C) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Same fragment restrains
{C1, C14, C2, C3, N2, C4, C5}
as
{C1B, C14B, C2B, C3B, N2B, C4B, C5B}
{C19, N5, C20, C21, C22, C23, C24, C25}
as
{C7, N3, C8, C9, C10, C11, C12, C13}
{C19, N5, C20, C21, C22, C23, C24, C25}
as
{C7B, N3B, C8B, C9B, C10B, C11B, C12B, C13B}
{C19, N5, C20, C21, C22, C23, C24, C25}
as
{C7C, N3C, C8C, C9C, C10C, C11C, C12C, C13C}
{C20, C21, C22, C23, C24, C25}
as
{C20B, C21B, C22B, C23B, C24B, C25B}
5. Others
 1*[Sof(C7)+Sof(H7)+Sof(N3)+Sof(H3)+Sof(C8)+Sof(H8)+Sof(C9)+Sof(H9A)+Sof(H9B)+
 Sof(C10)+Sof(H10A)+Sof(H10B)+Sof(C11)+Sof(H11A)+Sof(H11B)+Sof(C12)+Sof(H12A)+
 Sof(H12B)+Sof(C13)+Sof(H13A)+Sof(H13B)]+1*[Sof(C7B)+Sof(H7B)+Sof(N3B)+Sof(H3B)+
 Sof(C8B)+Sof(H8B)+Sof(C9B)+Sof(H9BA)+Sof(H9BB)+Sof(C10B)+Sof(H10C)+Sof(H10D)+
 Sof(C11B)+Sof(H11C)+Sof(H11D)+Sof(C12B)+Sof(H12C)+Sof(H12D)+Sof(C13B)+
 Sof(H13C)+Sof(H13D)]+1*[Sof(C7C)+Sof(H7C)+Sof(N3C)+Sof(H3C)+Sof(C8C)+Sof(H8C)+
 Sof(C9C)+Sof(H9CA)+Sof(H9CB)+Sof(C10C)+Sof(H10E)+Sof(H10F)+Sof(C11C)+Sof(H11E)+
 Sof(H11F)+Sof(C12C)+Sof(H12E)+Sof(H12F)+Sof(C13C)+Sof(H13E)+Sof(H13F)]=1 with
 esd of 0.001
 Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22C)=
 Sof(H22D)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=
 Sof(C25B)=Sof(H25C)=Sof(H25D)=1-FVAR(1)
 Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=FVAR(1)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C14B)=Sof(H14C)=Sof(H14D)=Sof(C2B)=
 Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(N2B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=1-
 FVAR(2)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(N2)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=FVAR(2)
 Sof(C7)=Sof(H7)=Sof(N3)=Sof(H3)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=
 Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=FVAR(3)
 Sof(C7B)=Sof(H7B)=Sof(N3B)=Sof(H3B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(H9BA)=
 Sof(H9BB)=Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11C)=Sof(H11D)=
 Sof(C12B)=Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13C)=Sof(H13D)=FVAR(4)
 Sof(C7C)=Sof(H7C)=Sof(N3C)=Sof(H3C)=Sof(C8C)=Sof(H8C)=Sof(C9C)=Sof(H9CA)=
 Sof(H9CB)=Sof(C10C)=Sof(H10E)=Sof(H10F)=Sof(C11C)=Sof(H11E)=Sof(H11F)=
 Sof(C12C)=Sof(H12E)=Sof(H12F)=Sof(C13C)=Sof(H13E)=Sof(H13F)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C8(H8), C8B(H8B), C8C(H8C), C20(H20), C20B(H20B)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C2(H2A,H2B), C14B(H14C,H14D), C2B(H2BA,H2BB), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C9B(H9BA,H9BB),
  C10B(H10C,H10D), C11B(H11C,H11D), C12B(H12C,H12D), C13B(H13C,H13D), C9C(H9CA,
 H9CB), C10C(H10E,H10F), C11C(H11E,H11F), C12C(H12E,H12F), C13C(H13E,H13F),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
  C21B(H21C,H21D), C22B(H22C,H22D), C23B(H23C,H23D), C24B(H24C,H24D), C25B(H25C,
 H25D)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C4B(H4B), C5B(H5B), C7(H7), N3(H3), C7B(H7B), N3B(H3B),
 C7C(H7C), N3C(H3C), C16(H16), C17(H17), C19(H19)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1B(H1BA,H1BB,H1BC)
;