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_7045936
_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 Fe2 Gd2 N28 O14, 6(H2 O)'
_chemical_formula_sum            'C40 H50 B2 Fe2 Gd2 N28 O20'
_chemical_formula_weight         1690.90
_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     dual
_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                61.132(5)
_cell_angle_beta                 77.180(5)
_cell_angle_gamma                67.107(4)
_cell_formula_units_Z            1
_cell_length_a                   10.9350(10)
_cell_length_b                   13.5290(12)
_cell_length_c                   13.8570(12)
_cell_measurement_reflns_used    3875
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      2.75
_cell_measurement_theta_min      25.10
_cell_volume                     1652.4(3)
_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_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1127
_diffrn_reflns_av_unetI/netI     0.1410
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10584
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_diffrn_reflns_theta_min         1.85
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.498
_exptl_absorpt_correction_T_max  0.8251
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.861
_refine_diff_density_min         -2.116
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         5400
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+30.3923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2086
_reflns_number_gt                4105
_reflns_number_total             5400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt00895g2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7045934--7045937.cif.'
_cod_database_code               7045936
_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. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O5W(0.6) H5WA(0.6) H5WB(0.6) O4W(0.5) H4WA(0.5) H4WB(0.5) O3W(0.5)
 H3WA(0.5) H3WB(0.5) O6W(0.4) H6WA(0.4) H6WB(0.4)
4.a Riding coordinates:
 O1W(H1WB,H1WA), O5W(H5WA,H5WB), O4W(H4WA,H4WB), O2W(H2WA,H2WB), O3W(H3WA,
 H3WB), O6W(H6WA,H6WB)
4.b Ternary CH refined with riding coordinates:
 B1(H1A)
4.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'