Electrochemical Evidence for Hemilabile Coordination of 1,3-Dimethyllumazine to [1,1′-Bis(diorganophosphino)ferrocene]copper(I)
Jana, Rajkumar; Sarkar, Biprajit; Strobel, Sabine; Mobin, Shaikh M.; Kaim, Wolfgang; Fiedler, Jan; Organometallics 33 (2014) 4784–; doi:10.1021/om500039a

data_4083135
_publ_section_title
;
 Electrochemical Evidence for Hemilabile Coordination of
 1,3-Dimethyllumazine to
 [1,1&#x2032;-Bis(diorganophosphino)ferrocene]copper(I)
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4784
_journal_paper_doi               10.1021/om500039a
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C30 H44 Cu Fe N4 O2 P2, B F4, C H2 Cl2'
_chemical_formula_sum            'C31 H46 B Cl2 Cu F4 Fe N4 O2 P2'
_chemical_formula_weight         845.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.9980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9608(3)
_cell_length_b                   11.7770(2)
_cell_length_c                   20.7616(4)
_cell_measurement_reflns_used    9204
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      0.41
_cell_volume                     3643.41(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17116
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.7653
_exptl_absorpt_correction_T_min  0.5592
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Scalepack (W. Minor & Z. Otwinowski)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'coarse shape'
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         8973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+2.1792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                6280
_reflns_number_total             8973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500039a_si_002.cif
_cod_data_source_block           rjmar09
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4083135