Solid-state <sup>45</sup>Sc NMR studies of Cp*<sub>2</sub>Sc-X and Cp*<sub>2</sub>ScX(THF).
Huynh, Winn; Culver, Damien B.; Tafazolian, Hosein; Conley, Matthew P.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13063–13071; doi:10.1039/c8dt02623h

data_7047324
_publ_section_title
;
 Solid-state <sup>45</sup>Sc NMR studies of Cp*<sub>2</sub>Sc-X and
 Cp*<sub>2</sub>ScX(THF).
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13063
_journal_page_last               13071
_journal_paper_doi               10.1039/c8dt02623h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C20 H30 Cl Sc'
_chemical_formula_weight         350.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1990(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.7408(8)
_cell_length_b                   21.3333(17)
_cell_length_c                   16.7347(13)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.35
_cell_measurement_theta_min      2.61
_cell_volume                     3834.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.002
_diffrn_measured_fraction_theta_max 1.002
_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_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 1.002
_diffrn_reflns_Laue_measured_fraction_max 1.002
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            91793
_diffrn_reflns_point_group_measured_fraction_full 1.002
_diffrn_reflns_point_group_measured_fraction_max 1.002
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.547
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prism frag'
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.139
_exptl_transmission_factor_max   0.942
_exptl_transmission_factor_min   0.854
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         23372
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0506P)^2^+1.7192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    1.002
_reflns_Friedel_fraction_max     1.002
_reflns_number_gt                19808
_reflns_number_total             23372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02623h2.cif
_cod_data_source_block           mc10wh_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7047321--7047324.cif.
;
_cod_database_code               7047324
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.931
_shelxl_version_number           2013-4
_shelx_res_checksum              95539