Interligand C-C Coupling between α-Methyl N-Heterocycles and bipy or phen at Rhenium Tricarbonyl Complexes.
Arévalo, Rebeca; Riera, Lucía; Pérez, Julio; Inorganic chemistry 56 (2017) 4249–4252; doi:10.1021/acs.inorgchem.7b00078

data_4345801
_publ_section_title
;
 Interligand C-C Coupling between \a-Methyl N-Heterocycles and bipy or
 phen at Rhenium Tricarbonyl Complexes.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4249
_journal_page_last               4252
_journal_paper_doi               10.1021/acs.inorgchem.7b00078
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_sum            'C25 H23 N4 O3 Re'
_chemical_formula_weight         613.67
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   10.5338(1)
_cell_length_b                   14.2032(2)
_cell_length_c                   15.2605(2)
_cell_measurement_reflns_used    9033
_cell_measurement_temperature    130.0(1)
_cell_measurement_theta_max      69.1540
_cell_measurement_theta_min      4.1610
_cell_volume                     2283.18(5)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12044
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.223
_diffrn_reflns_theta_min         4.252
_diffrn_source                   'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+4.8445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3982
_reflns_number_total             4077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00078_si_001.cif
_cod_data_source_block           compound_13
_cod_original_cell_volume        2283.20(5)
_cod_database_code               4345801
_shelxl_version_number           2014-3
_shelx_res_checksum              36489
_shelx_hkl_checksum              168