Metallacyclic Zinc Complexes of Alkylidene-Linked Bitopic Bis(pyrazolyl)methane Ligands: Unusual Exocyclic Bridging Fluoride Ligands
Reger, Daniel L.; Watson, Russell P.; Smith, Mark D.; Pellechia, Perry J.; Crystal Growth & Design 7 (2007) 1163–; doi:10.1021/cg070078s

data_4504224
_publ_section_title
;
 Metallacyclic Zinc Complexes of Alkylidene-Linked Bitopic
 Bis(pyrazolyl)methane Ligands:&#x00A0; Unusual Exocyclic Bridging
 Fluoride Ligands
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1163
_journal_paper_doi               10.1021/cg070078s
_journal_volume                  7
_journal_year                    2007
_chemical_formula_moiety         'C51 H70 N24 O5 Zn3, 4(C2 H3 N), 6(B F4)'
_chemical_formula_sum            'C59 H82 B6 F24 N28 O5 Zn3'
_chemical_formula_weight         1980.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.2860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.5797(12)
_cell_length_b                   15.8645(9)
_cell_length_c                   28.6555(17)
_cell_measurement_reflns_used    5639
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      23.005
_cell_measurement_theta_min      2.235
_cell_volume                     9299.4(9)
_computing_cell_refinement       'SAINT+ NT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART NT V5.625 (Bruker, 1998)'
_computing_data_reduction        'SAINT+ NT V6.22'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39096
_diffrn_reflns_theta_full        22.54
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         6093
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0694
_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^)+(0.1467P)^2^+4.3686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2133
_reflns_number_gt                4802
_reflns_number_total             6093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg070078ssi20070307_122135.cif
_cod_data_source_block           3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4504224