Monomeric, Tetrameric, and Polymeric Copper Di-tert-butyl Phosphate Complexes Containing Pyridine Ancillary Ligands
Ramaswamy Murugavel; Malaichamy Sathiyendiran; Ramasamy Pothiraja; Mrinalini G. Walawalkar; Talal Mallah; Eric Riviére; Inorganic Chemistry 43 (2004) 945–953; doi:10.1021/ic0349508

data_4310521
_publ_section_title
;
 Monomeric, Tetrameric, and Polymeric Copper Di-tert-butyl Phosphate
 Complexes Containing Pyridine Ancillary Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              945
_journal_page_last               953
_journal_paper_doi               10.1021/ic0349508
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C58 H120 Cu4 N2 O26 P6'
_chemical_formula_weight         1701.54
_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                 94.14(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.741(2)
_cell_length_b                   16.6507(10)
_cell_length_c                   22.6728(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.81
_cell_measurement_theta_min      11.31
_cell_volume                     8562.7(12)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega 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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7716
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  0.7605
_exptl_absorpt_correction_T_min  0.6543
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.424
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         7515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0852P)^2^+32.5949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1765
_reflns_number_gt                4981
_reflns_number_total             7515
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0349508si20031012_070004_2.cif
_cod_data_source_block           rm078b(tetramer)
_cod_original_cell_volume        8562.6(11)
_cod_database_code               4310521