Synthesis of a sumanenyl hafnocene complex
Amaya, Toru; Katoh, Shun; Moriuchi, Toshiyuki; Hirao, Toshikazu; Organic Chemistry Frontiers 6 (2019) 1032–; doi:10.1039/C9QO00140A

data_1554742
_publ_section_title
;
 Synthesis of a sumanenyl hafnocene complex
;
_journal_issue                   7
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1032
_journal_paper_doi               10.1039/C9QO00140A
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C31 H26 Cl2 Hf'
_chemical_formula_sum            'C31 H26 Cl2 Hf'
_chemical_formula_weight         647.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-01-25 deposited with the CCDC.	2019-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.0903(16)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   8.1722(5)
_cell_length_b                   16.0848(7)
_cell_length_c                   9.1272(6)
_cell_measurement_reflns_used    9342
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.21
_cell_volume                     1195.02(12)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11659
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         3.208
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.599
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             636.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.85
_refine_diff_density_min         -1.71
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2822
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0087P)^2^+5.3003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2442
_reflns_number_total             2822
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c9qo00140a2.cif
_cod_data_source_block           131219SuHfCl2CpMe5
_cod_original_cell_volume        1195.02(11)
_cod_database_code               1554742
_shelx_res_checksum              37742
_shelx_hkl_checksum              86884