Improved syntheses, and structural and electronic characterization of carboxamide-substituted Tp^CONHPh,Me^ and Tp^CONH<i>t^-Bu,Me</i> ligands
Sirianni, Eric R.; Yap, Glenn P. A.; Akturk, Eser S.; Theopold, Klaus H.; Acta Crystallographica Section C 69 (2013) 947–953; doi:10.1107/S0108270113015898

data_2019121
_publ_section_title
;
 Improved syntheses, and structural and electronic characterization of
 carboxamide-substituted Tp^CONHPh,Me^ and Tp^CONH<i>t^-Bu,Me</i> ligands
;
_journal_coeditor_code           EG3122
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              947
_journal_page_last               953
_journal_paper_doi               10.1107/S0108270113015898
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Cu (C27 H43 B N9 O3) (C O)] , 0.5C4 H8 O'
_chemical_formula_moiety         'C28 H43 B Cu N9 O4, 0.5(C4 H8 O)'
_chemical_formula_sum            'C30 H47 B Cu N9 O4.5'
_chemical_formula_weight         680.12
_chemical_name_systematic
'Carbonyl[tris(3-<i>tert</i>-butylaminocarbonyl-5-methylpyrazol-1-yl-\k<i>N</i>^2^)borato]copper(I) tetrahydrofuran hemisolvate'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.1972(11)
_cell_length_b                   15.7870(11)
_cell_length_c                   34.902(3)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.89
_cell_measurement_theta_min      2.20
_cell_volume                     8373.6(11)
_computing_cell_refinement       'APEX2 (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'APEX2 (Bruker, 2007)'
_computing_molecular_graphics    'APEX2 (Bruker, 2007)'
_computing_publication_material  'APEX2 (Bruker, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            92865
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.9346
_exptl_absorpt_correction_T_min  0.7925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(APEX2; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.343
_refine_ls_abs_structure_details
;
 Flack x determined using 5516 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.009(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         19225
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0782P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                14552
_reflns_number_total             19225
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3122.cif
_cod_data_source_block           V
_cod_original_cell_volume        8373.6(10)
_cod_original_formula_sum        'C30 H47 B Cu N9 O4.50'
_cod_database_code               2019121
_cod_database_fobs_code          2019121
_shelxl_version_number           20.13