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_4323228
_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            'C40.5 H39.5 Cu F3 N6 O9.5 S'
_chemical_formula_weight         914.89
_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                103.11(3)
_cell_angle_beta                 110.08(3)
_cell_angle_gamma                102.78(3)
_cell_formula_units_Z            2
_cell_length_a                   12.509(4)
_cell_length_b                   12.716(4)
_cell_length_c                   14.889(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203.2
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      10.3
_cell_volume                     2047.3(14)
_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
_diffrn_ambient_temperature      203.2
_diffrn_measurement_device       unknown
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.03729
_diffrn_orient_matrix_UB_12      -0.02925
_diffrn_orient_matrix_UB_13      0.05598
_diffrn_orient_matrix_UB_21      0.08141
_diffrn_orient_matrix_UB_22      0.05170
_diffrn_orient_matrix_UB_23      0.01501
_diffrn_orient_matrix_UB_31      -0.00974
_diffrn_orient_matrix_UB_32      0.06152
_diffrn_orient_matrix_UB_33      0.04882
_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  0.02360
_diffrn_reflns_limit_h_max       -100
_diffrn_reflns_limit_h_min       100
_diffrn_reflns_limit_k_max       -100
_diffrn_reflns_limit_k_min       100
_diffrn_reflns_limit_l_max       -100
_diffrn_reflns_limit_l_min       100
_diffrn_reflns_number            7532
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -4.51
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             945.00
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_refine_diff_density_max         0.71
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.330
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     559
_refine_ls_number_reflns         5301
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0610
_refine_ls_shift/su_max          0.6990
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00024|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0900
_reflns_number_gt                5301
_reflns_number_total             7176
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic9713487_07.cif
_cod_data_source_block           '_[(L2)2Cu](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_cell_volume        2047(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C40.50 H39.50 Cu F3 N6 O9.50 S '
_cod_database_code               4323228