A study of di(amino)stibines with terminal Sb(iii) hydrogen-ligands by X-ray- and neutron-diffraction.
Schwamm, Ryan J.; Edwards, Alison J.; Fitchett, Christopher M.; Coles, Martyn P.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 2953–2958; doi:10.1039/c8dt05113e

data_7048826
_publ_section_title
;
 A study of di(amino)stibines with terminal Sb(iii) hydrogen-ligands by
 X-ray- and neutron-diffraction.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2953
_journal_page_last               2958
_journal_paper_doi               10.1039/c8dt05113e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C20 H31 N2 O1 Sb1 Si2'
_chemical_formula_sum            'C20 H31 N2 O Sb Si2'
_chemical_formula_weight         493.40
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2019-01-30 deposited with the CCDC.
2019-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                99.459(5)
_cell_angle_beta                 100.012(5)
_cell_angle_gamma                107.557(6)
_cell_formula_units_Z            2
_cell_length_a                   7.6028(5)
_cell_length_b                   11.5896(8)
_cell_length_c                   13.8020(7)
_cell_measurement_reflns_used    5427
_cell_measurement_temperature    120
_cell_measurement_theta_max      29
_cell_measurement_theta_min      4
_cell_volume                     1110.98(13)
_computing_cell_refinement       'LaueG (Piltz, 2011)'
_computing_data_collection       'MAATEL/ANSTO control program'
_computing_data_reduction
'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution
'heavy atom positions from X-ray\^A diffraction used as starting model for neutronstructure refinement\'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.775
_diffrn_measured_fraction_theta_max 0.775
_diffrn_measurement_details      '20 images, exposure time   100 minutes'
_diffrn_measurement_device       'Laue image-plate diffractometer'
_diffrn_measurement_device_type  KOALA
_diffrn_measurement_method       Laue
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.85
_diffrn_reflns_av_R_equivalents  0.079
_diffrn_reflns_av_unetI/netI     0.2989
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9118
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_theta_full        57.80
_diffrn_reflns_theta_max         57.91
_diffrn_reflns_theta_min         0.000
_diffrn_source                   'nuclear reactor'
_diffrn_source_details           'thermal neutrons, supermirror guides'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             108
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.4721
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         875
_refine_ls_number_restraints     288
_refine_ls_R_factor_all          0.1572
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.0007899
_refine_ls_shift/su_mean         0.0000893
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 5.48 -4.54 2.29 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1429
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0537
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                1031
_reflns_number_total             1801
_reflns_threshold_expression     >2sigma(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0509
_oxford_refine_ls_scale          0.771(7)
_oxford_reflns_number_all        1796
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c8dt05113e2.cif
_cod_data_source_block           Compound-2a-neutron
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 7048824--7048828.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C20 H31 N2 O1 Sb1 Si2'
_cod_database_code               7048826