Syntheses and structures of the first examples of zinc compounds with bridging fluorine and hydrogen atoms
Hao, Haijun; Cui, Chunming; Roesky, Herbert W.; Bai, Guangcai; Schmidt, Hans-Georg; Noltemeyer, Mathias; Chemical Communications  (2001) 1118–; doi:10.1039/b102275j

data_7114893
_publ_section_title
;
 Syntheses and structures of the first examples of zinc compounds with
 bridging fluorine and hydrogen atoms
;
_journal_issue                   12
_journal_name_full               'Chemical Communications'
_journal_page_first              1118
_journal_paper_doi               10.1039/b102275j
_journal_year                    2001
_chemical_formula_sum            'C48 H58 N4 Zn2'
_chemical_formula_weight         821.72
_chemical_name_systematic        ?
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.941(5)
_cell_length_b                   20.576(3)
_cell_length_c                   24.918(4)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     8686(3)
_computing_cell_refinement       'STOE DIF4'
_computing_data_collection       'STOE DIF4'
_computing_data_reduction        'STOE REDU4'
_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      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE AED2 four circle diffractometer'
_diffrn_measurement_method       'profile fitted theta omega 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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            3065
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.52
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.5993
_exptl_absorpt_correction_T_min  0.4622
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                1699
_reflns_number_total             1915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102275j.txt
_cod_data_source_block           roe909b
_cod_original_sg_symbol_H-M      Fddd
_cod_original_formula_sum        'C48 H58 N4 Zn2 incl. benzene'
_cod_database_code               7114893
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C48 H58 N4 Zn2 be cl e en in nz' to 'C48 H58 N4 Zn2'.

 Antanas Vaitkus,
 2017-01-07
;