Dynamic Topochemical Reaction Control−A Principle and Its Application inansa-Metallocene Synthesis†
Greger, Ingo; Kehr, Gerald; Fröhlich, Roland; Erker, Gerhard; Organometallics 29 (2010) 3210–; doi:10.1021/om100467y

data_4066459
_publ_section_title
;
 Dynamic Topochemical Reaction Control&#x2212;A Principle and Its
 Application inansa-Metallocene Synthesis&#x2020;
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3210
_journal_paper_doi               10.1021/om100467y
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C18 H22 Cl2 Zr'
_chemical_formula_weight         400.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.369(2)
_cell_angle_beta                 86.137(2)
_cell_angle_gamma                66.616(1)
_cell_formula_units_Z            6
_cell_length_a                   12.4775(4)
_cell_length_b                   14.3156(5)
_cell_length_c                   16.5925(6)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      0.41
_cell_volume                     2642.61(16)
_computing_cell_refinement       'APEX2 (BrukerAXS, 2006)'
_computing_data_collection       'APEX2 (BrukerAXS, 2006)'
_computing_data_reduction        'APEX2 (BrukerAXS, 2006)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46260
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.9730
_exptl_absorpt_correction_T_min  0.8376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (BrukerAXS, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.245
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         13002
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0922P)^2^+10.9458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1974
_refine_ls_wR_factor_ref         0.2470
_reflns_number_gt                6743
_reflns_number_total             13002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100467y_si_002.cif
_cod_data_source_block           erk5131
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4066459