Magnetic Ordering in Two Molecule-Based (10,3)-a Nets Prepared from a Copper(II) Trinuclear Secondary Building Unit
Beatriz Gil-Hernández; Pedro Gili; Jana K. Vieth; Christoph Janiak; Joaquín Sanchiz; Inorganic Chemistry 49 (2010) 7478–7490; doi:10.1021/ic100796e

data_4316270
_publ_section_title
;
 Magnetic Ordering in Two Molecule-Based (10,3)-a Nets Prepared from a
 Copper(II) Trinuclear Secondary Building Unit
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7478
_journal_page_last               7490
_journal_paper_doi               10.1021/ic100796e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C9 H3 Cl Cu3 Mn O18, 2(C24 H20 P), O'
_chemical_formula_sum            'C57 H43 Cl Cu3 Mn O19 P2'
_chemical_formula_weight         1374.86
_chemical_name_systematic
; 
catena-{bis(tetraphenylphosphonium)[\m3-chloro-tris-\m3-mesoxalato-
-\kO:O',O'':O'',O''':O''''-triscuprate(II)-manganate(II)} monohydrate 
(Ph4P)2[MnCu3(mesox)3Cl].H2o
with H2 on crystal water included for calculation:
C57 H45 Cl Cu3 Mn O19 P2, M = 1376.88
Z = 4, F(000) = 2792, Dx = 1.605 g/cm-3
 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.963(3)
_cell_length_b                   18.283(3)
_cell_length_c                   18.373(3)
_cell_measurement_reflns_used    3278
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      16.7
_cell_measurement_theta_min      2.2
_cell_volume                     5698.1(17)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX2 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_sigmaI/netI    0.0940
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19510
_diffrn_reflns_theta_full        20.03
_diffrn_reflns_theta_max         20.03
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  0.6375
_exptl_absorpt_correction_T_min  0.5331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         5328
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0967P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1643
_reflns_number_gt                3972
_reflns_number_total             5328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100796e_si_002_2.cif
_cod_data_source_block           Comp2
_cod_original_cell_volume        5698.2(15)
_cod_database_code               4316270