Unprecedented Mixed-Valence Cu(I)/Cu(II) Complex Derived fromN-Methyl-1,3,5-triaza-7-phosphaadamantane: Synthesis, Structural Features, and Magnetic Properties
Kirillov, Alexander M.; Filipowicz, Małgorzata; Guedes da Silva, M. Fátima C.; Kłak, Julia; Smoleński, Piotr; Pombeiro, Armando J. L.; Organometallics 31 (2012) 7921–; doi:10.1021/om3005564

data_4079189
_publ_section_title
;
 Unprecedented Mixed-Valence Cu(I)/Cu(II) Complex Derived
 fromN-Methyl-1,3,5-triaza-7-phosphaadamantane: Synthesis, Structural
 Features, and Magnetic Properties
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              7921
_journal_paper_doi               10.1021/om3005564
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C28 H60 Cu4 I4 N30 P4, 2(H2 O)'
_chemical_formula_sum            'C28 H64 Cu4 I4 N30 O2 P4'
_chemical_formula_weight         1738.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                109.430(8)
_cell_angle_beta                 101.394(5)
_cell_angle_gamma                98.230(7)
_cell_formula_units_Z            1
_cell_length_a                   7.589(4)
_cell_length_b                   13.7459(12)
_cell_length_c                   14.8097(18)
_cell_measurement_reflns_used    5749
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.59
_cell_volume                     1391.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12877
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    3.903
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+2.7680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                4316
_reflns_number_total             5054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3005564_si_002.cif
_cod_data_source_block           Piotr050810
_cod_original_cell_volume        1391.2(8)
_cod_database_code               4079189