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_7045937
_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         'C56 H48 B2 Fe2 La2 N34 O11, 10(O)'
_chemical_formula_sum            'C56 H48 B2 Fe2 La2 N34 O22'
_chemical_formula_weight         1960.42
_chemical_properties_physical    Air-sensitive
_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
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-11-13 deposited with the CCDC.
2018-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                89.017(6)
_cell_angle_beta                 77.566(6)
_cell_angle_gamma                89.386(6)
_cell_formula_units_Z            1
_cell_length_a                   12.0687(9)
_cell_length_b                   13.3292(10)
_cell_length_c                   13.3974(8)
_cell_measurement_reflns_used    3168
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.0260
_cell_measurement_theta_min      2.1940
_cell_volume                     2104.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SuperFlip (Palatinus & Chapius, 2007)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'KappaCCD 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_UB_11      -0.0217718
_diffrn_orient_matrix_UB_12      0.0726326
_diffrn_orient_matrix_UB_13      -0.0021773
_diffrn_orient_matrix_UB_21      -0.0774066
_diffrn_orient_matrix_UB_22      -0.0196007
_diffrn_orient_matrix_UB_23      -0.0085678
_diffrn_orient_matrix_UB_31      -0.0280047
_diffrn_orient_matrix_UB_32      -0.0013858
_diffrn_orient_matrix_UB_33      0.0764462
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1299
_diffrn_reflns_av_unetI/netI     0.1171
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36885
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.198
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44620
_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            brown
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       plate
_exptl_crystal_F_000             974
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.443
_refine_diff_density_min         -1.530
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         8561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6125
_reflns_number_total             8561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00895g2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7045934--7045937.cif.'
_cod_database_code               7045937
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.794
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              38435