Syntheses and characterization of hepta-coordinated Group 4 amidinate complexes.
Cook, Tabitha M.; Steren, Carlos A.; Xue, Zi-Ling; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11030–11040; doi:10.1039/c8dt02523a

data_7047033
_publ_section_title
;
 Syntheses and characterization of hepta-coordinated Group 4 amidinate
 complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11030
_journal_page_last               11040
_journal_paper_doi               10.1039/c8dt02523a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C24 H51 Cl Hf N6'
_chemical_formula_sum            'C24 H51 Cl Hf N6'
_chemical_formula_weight         637.64
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-09 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.053(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4324(15)
_cell_length_b                   16.447(2)
_cell_length_c                   17.091(2)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.24
_cell_volume                     2928.3(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6975
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.610
_diffrn_reflns_theta_min         1.720
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.675
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 52071 reflections, Rint = 0.0575
 (28386 with I > 3sig(I), Rint = 0.0487)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.233
_refine_diff_density_max         5.326
_refine_diff_density_min         -2.240
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+19.3454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6152
_reflns_number_total             6975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02523a2.cif
_cod_data_source_block           HfAmid3Cl
_cod_depositor_comments
'Adding full bibliography for 7047032--7047035.cif.'
_cod_original_cell_volume        2928.3(7)
_cod_database_code               7047033
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6703(13)
 0.3297(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C22(H22), C19(H19), C14(H14), C11(H11), C6(H6), C3(H3)
3.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C21(H21A,H21B,H21C), C2(H2A,H2B,H2C), C24(H24A,H24B,
 H24C), C23(H23A,H23B,H23C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C),
 C20(H20A,H20B,H20C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              37966
_olex2_submission_special_instructions 'No special instructions were received'