Design of 3d-4f molecular squares through the [Fe{(HB(pz)<sub>3</sub>)}(CN)<sub>3</sub>]<sup>-</sup> metalloligand.
Alexandru, Maria-Gabriela; Visinescu, Diana; Shova, Sergiu; Oliveira, Willian X. C.; Lloret, Francesc; Julve, Miguel; Dalton transactions (Cambridge, England : 2003) 47 (2018) 6005–6017; doi:10.1039/c8dt00895g

data_7045934
_publ_section_title
;
 Design of 3d-4f molecular squares through the
 [Fe{(HB(pz)<sub>3</sub>)}(CN)<sub>3</sub>]<sup>-</sup> metalloligand.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6005
_journal_page_last               6017
_journal_paper_doi               10.1039/c8dt00895g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C40 H38 B2 Dy2 Fe2 N28 O14, 4(H2 O)'
_chemical_formula_sum            'C40 H46 B2 Dy2 Fe2 N28 O18'
_chemical_formula_weight         1665.37
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-10-27 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                61.208(8)
_cell_angle_beta                 77.217(7)
_cell_angle_gamma                66.516(8)
_cell_formula_units_Z            1
_cell_length_a                   11.0216(9)
_cell_length_b                   13.5484(8)
_cell_length_c                   13.8450(11)
_cell_measurement_reflns_used    4009
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6600
_cell_measurement_theta_min      1.7740
_cell_volume                     1660.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -19.00  18.00   1.00   60.00    --  -15.44 -99.00 -90.00   37
  2  \w    -22.00  24.00   1.00   60.00    --  -15.44 -99.00 150.00   46
  3  \w    -33.00  38.00   1.00   60.00    --   17.71 -77.00   0.00   71
  4  \w     43.00  85.00   1.00   60.00    --   17.71  38.00 -30.00   42
  5  \w     12.00  85.00   1.00   60.00    --   17.71  57.00-180.00   73
  6  \w     35.00  84.00   1.00   60.00    --   17.71 178.00   0.00   49
  7  \w      0.00  87.00   1.00   60.00    --   17.71  38.00 120.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0680159000
_diffrn_orient_matrix_UB_12      -0.0266327000
_diffrn_orient_matrix_UB_13      0.0123589000
_diffrn_orient_matrix_UB_21      -0.0171448000
_diffrn_orient_matrix_UB_22      -0.0267042000
_diffrn_orient_matrix_UB_23      0.0570373000
_diffrn_orient_matrix_UB_31      0.0033084000
_diffrn_orient_matrix_UB_32      -0.0511414000
_diffrn_orient_matrix_UB_33      -0.0042144000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12061
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.735
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.422
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                4933
_reflns_number_total             5818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt00895g2.cif
_cod_data_source_block           shi_3469_divi
_cod_depositor_comments
'Adding full bibliography for 7045934--7045937.cif.'
_cod_original_cell_volume        1660.7(2)
_cod_database_code               7045934
_chemical_oxdiff_formula         'C30 H30 N8 O8 Fe1 Dy1'
_chemical_oxdiff_usercomment     FeDypyim
_reflns_odcompleteness_completeness 99.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O5W(0.15) H5WA(0.15) H5WB(0.15) O6W(0.25) H6WA(0.25) H6WB(0.25)
 O4W(0.4) H4WA(0.4) H4WB(0.4) O7W(0.25) H7WA(0.25) H7WB(0.25) O2W(0.2)
 H2WA(0.2) H2WB(0.2) O3W(0.75) H3WA(0.75) H3WB(0.75)
3.a Riding coordinates:
 O1W(H1WA,H1WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB), O4W(H4WA,H4WB), O7W(H7WA,
 H7WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
3.b Ternary CH refined with riding coordinates:
 B1(H1A)
3.c Aromatic/amide H refined with riding coordinates:
 N11(H11), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8),
 C9(H9), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.676
_oxdiff_exptl_absorpt_empirical_full_min 0.764