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_7032824
_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 Fe N5, C6 H6'
_chemical_formula_sum            'C31 H43 Cl2 Fe N5'
_chemical_formula_weight         612.45
_chemical_name_systematic
;
 ?
;
_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
_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                 93.857(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5749(7)
_cell_length_b                   16.7758(9)
_cell_length_c                   12.7588(8)
_cell_measurement_temperature    100(2)
_cell_volume                     3112.5(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47034
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.124
_diffrn_reflns_theta_min         2.386
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.8322
_exptl_absorpt_correction_T_min  0.6405
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.713
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.278
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         6881
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0244P)^2^+7.6214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5903
_reflns_number_total             6881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02327g2.cif
_cod_data_source_block           cd11e
_cod_depositor_comments
'Adding full bibliography for 7032823--7032828.cif.'
_cod_database_code               7032824
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.641
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C40B \\sim C41B
\\sim C42B \\sim C43B \\sim C44B \\sim C45B: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Same fragment restrains
{C40, C41, C42, C43, C44, C45}
as
{C40B, C41B, C42B, C43B, C44B, C45B}
4. Others
 Sof(C40B)=Sof(H40B)=Sof(C41B)=Sof(H41B)=Sof(C42B)=Sof(H42B)=Sof(C43B)=
 Sof(H43B)=Sof(C44B)=Sof(H44B)=Sof(C45B)=Sof(H45B)=1-FVAR(1)
 Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=Sof(C43)=Sof(H43)=
 Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C20(H20)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
  C24(H24A,H24B), C25(H25A,H25B)
5.c Me refined with riding coordinates:
 C1(H1A,H1B,H1C)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5A), C7(H7), C16(H16), C17(H17), C19(H19), C40(H40), C41(H41),
 C42(H42), C43(H43), C44(H44), C45(H45), C40B(H40B), C41B(H41B), C42B(H42B),
 C43B(H43B), C44B(H44B), C45B(H45B)
;