Self-assembly of metallomacrocycles with dipyrazole ligands and anion sensing of [Pd4Fe2] macrocycle with ferrocene-based dipyrazole ligand
Yao, Liao-Yuan; Yu, Zheng-Su; Qin, Lin; Li, Yi-Zhi; Qin, Yu; Yu, Shu-Yan; Dalton Transactions 42 (2013) 3447–; doi:10.1039/c2dt32576d

data_7020944
_publ_section_title
;
 Self-assembly of metallomacrocycles with dipyrazole ligands and anion
 sensing of [Pd4Fe2] macrocycle with ferrocene-based dipyrazole ligand
;
_journal_issue                   10
_journal_name_full               'Dalton Transactions'
_journal_page_first              3447
_journal_paper_doi               10.1039/c2dt32576d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety
'C94 H76 N16 O2 Pd4, 4.2(H2 O), 4(N O3), 2(H0.80 O0.40)'
_chemical_formula_sum            'C94 H86 N20 O19 Pd4'
_chemical_formula_weight         2225.43
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.539(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   40.030(3)
_cell_length_b                   12.6014(18)
_cell_length_c                   21.3785(15)
_cell_measurement_reflns_used    4036
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      21.35
_cell_measurement_theta_min      2.20
_cell_volume                     10773.5(19)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36308
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.8564
_exptl_absorpt_correction_T_min  0.8223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs; bRUKER, 2000'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4504
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         10593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0651
_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^)+(0.06P)^2^+1.55P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                7348
_reflns_number_total             10593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32576d.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed
to 'constr' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        10773.6(19)
_cod_original_sg_symbol_H-M      'C2/c '
_cod_database_code               7020944