Synthesis and Characterization of a Family of Systematically Varied Tris(2-pyridyl)methoxymethane Ligands: Copper(I) and Copper(II) Complexes
Robert T. Jonas; T. D. P. Stack; Inorganic Chemistry 37 (1998) 6615–6629; doi:10.1021/ic9713487

data_4323225
_publ_contact_author
;
T. D. P. Stack
Department of Chemistry
Stanford University
Stanford, CA 94305
;
_publ_contact_author_email       ' STACK@LELAND.STANFORD.EDU '
_publ_contact_author_fax         ' (650) 725-0259 '
_publ_contact_author_phone       ' (650) 725-8736 '
_publ_section_title
;
 Synthesis and Characterization of a Family of Systematically Varied
 Tris(2-pyridyl)methoxymethane Ligands: Copper(I) and Copper(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6615
_journal_page_last               6629
_journal_paper_doi               10.1021/ic9713487
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C42 H8 Cu F3 N3 O8 P S'
_chemical_formula_weight         866.12
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                78.01(3)
_cell_angle_beta                 85.02(3)
_cell_angle_gamma                89.19(3)
_cell_formula_units_Z            4
_cell_length_a                   14.855(5)
_cell_length_b                   16.613(5)
_cell_length_c                   17.129(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203.2
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      9.9
_cell_volume                     4119(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution
;
SAPI91 (Fan, 1991)
;
_diffrn_ambient_temperature      203.2
_diffrn_measurement_device       unknown
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      -0.03669
_diffrn_orient_matrix_UB_12      0.01453
_diffrn_orient_matrix_UB_13      0.04685
_diffrn_orient_matrix_UB_21      -0.04567
_diffrn_orient_matrix_UB_22      0.02718
_diffrn_orient_matrix_UB_23      -0.03639
_diffrn_orient_matrix_UB_31      -0.03361
_diffrn_orient_matrix_UB_32      -0.05326
_diffrn_orient_matrix_UB_33      0.00855
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7109
_diffrn_reflns_av_R_equivalents  0.05720
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14091
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         23.41
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -1.14
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1728.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.52
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.780
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         7560
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.8020
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00005|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0620
_reflns_number_gt                7560
_reflns_number_total             12041
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic9713487_04.cif
_cod_data_source_block           '_[(L3)(PPh3)Cu](OTf)0.5(acetone)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C42 H8 Cu F3 N3 O8 P S '
_cod_database_code               4323225