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_4323232
_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            'C45 H48 Cu F6 N6 O15 S2'
_chemical_formula_weight         1154.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.01(5)
_cell_angle_beta                 96.02(4)
_cell_angle_gamma                90.12(5)
_cell_formula_units_Z            4
_cell_length_a                   14.949(7)
_cell_length_b                   20.54(1)
_cell_length_c                   16.461(7)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    273.2
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      10.3
_cell_volume                     5027(4)
_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      273.2
_diffrn_measurement_device       unknown
_diffrn_orient_matrix_UB_11      0.02274
_diffrn_orient_matrix_UB_12      -0.01727
_diffrn_orient_matrix_UB_13      -0.05079
_diffrn_orient_matrix_UB_21      0.00685
_diffrn_orient_matrix_UB_22      0.04550
_diffrn_orient_matrix_UB_23      -0.02006
_diffrn_orient_matrix_UB_31      0.06294
_diffrn_orient_matrix_UB_32      0.00136
_diffrn_orient_matrix_UB_33      0.02735
_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  0.03769
_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            9450
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -17.01
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      ?
_exptl_crystal_description       cubic
_exptl_crystal_F_000             2380.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.98
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.530
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     676
_refine_ls_number_reflns         5963
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.0850
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                5963
_reflns_number_total             9146
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic9713487_11.cif
_cod_data_source_block           '_[(L3)2Cu](OTf)2(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 21/n '
_cod_original_formula_sum        'C45 H48 Cu F6 N6 O15 S2 '
_cod_database_code               4323232