Unsymmetrical Zirconacyclopentadienes from Isolated Zirconacyclopropenes with 1-Alkynylphosphine Ligands
Miller, Adam D.; Johnson, Samuel A.; Tupper, Karl A.; McBee, Jennifer L.; Tilley, T. Don; Organometallics 28 (2009) 1252–; doi:10.1021/om801040t

data_4068699
_publ_section_title
;
 Unsymmetrical Zirconacyclopentadienes from Isolated Zirconacyclopropenes
 with 1-Alkynylphosphine Ligands
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1252
_journal_paper_doi               10.1021/om801040t
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C36 H35 P Zr'
_chemical_formula_sum            'C36 H35 P Zr'
_chemical_formula_weight         589.83
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.40(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.784(6)
_cell_length_b                   9.968(2)
_cell_length_c                   19.424(4)
_cell_measurement_reflns_used    1357
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      19.3
_cell_measurement_theta_min      3.44
_cell_volume                     5731(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0766
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14794
_diffrn_reflns_theta_full        20.90
_diffrn_reflns_theta_max         20.90
_diffrn_reflns_theta_min         3.34
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs, 2004'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         5719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0546P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                3598
_reflns_number_total             5719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801040t_si_006.cif
_cod_data_source_block           monom
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4068699