Synthetic, structural and reaction chemistry of N-heterocyclic germylene and stannylene compounds featuring N-boryl substituents.
Kristinsdóttir, Lilja; Oldroyd, Nicola L.; Grabiner, Rachel; Knights, Alastair W.; Heilmann, Andreas; Protchenko, Andrey V.; Niu, Haoyu; Kolychev, Eugene L.; Campos, Jesús; Hicks, Jamie; Christensen, Kirsten E.; Aldridge, Simon; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11951–11960; doi:10.1039/c9dt02449b

data_7701708
_publ_section_title
;
 Synthetic, structural and reaction chemistry of N-heterocyclic germylene
 and stannylene compounds featuring N-boryl substituents.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11951
_journal_page_last               11960
_journal_paper_doi               10.1039/c9dt02449b
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C54 H78 B2 N6'
_chemical_formula_sum            'C54 H78 B2 N6'
_chemical_formula_weight         832.87
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2015-11-30
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
;
2019-06-09 deposited with the CCDC.	2019-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.5685(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2417(2)
_cell_length_b                   22.3662(4)
_cell_length_c                   16.4812(3)
_cell_measurement_reflns_used    11375
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5204.07(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            89752
_diffrn_reflns_theta_full        26.659
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         5.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9471
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         12110
_refine_ls_number_restraints     163
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.0244551
_refine_ls_shift/su_mean         0.0006390
_refine_ls_structure_factor_coef Fsqd
_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: 
 21.8 31.7 15.5 3.82 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1562
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1562
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                8834
_reflns_number_total             12111
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.04
_oxford_diffrn_Wilson_scale      7.96
_oxford_refine_ls_r_factor_ref   0.0908
_oxford_refine_ls_scale          0.3607(4)
_oxford_reflns_number_all        12111
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 074noek15
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
SAME  C(13)  C(17)  C(16)  C(12)  AND 
CONT  C(13)  C(16)  C(12)  C(17)  AND 
CONT  C(13)  C(12)  C(17)  C(16)  AND 
CONT  C(14)  C(18)  C(15)  C(12)  AND 
CONT  C(14)  C(15)  C(12)  C(18)  AND 
CONT  C(14)  C(12)  C(18)  C(15) 
SIMU 0.01   C(13)  C(17)  C(16)  C(12)  AND 
CONT  C(13)  C(16)  C(12)  C(17)  AND 
CONT  C(13)  C(12)  C(17)  C(16)  AND 
CONT  C(14)  C(18)  C(15)  C(12)  AND 
CONT  C(14)  C(15)  C(12)  C(18)  AND 
CONT  C(14)  C(12)  C(18)  C(15) 
DELU 0.01   C(13)  C(17)  C(16)  C(12)  AND 
CONT  C(13)  C(16)  C(12)  C(17)  AND 
CONT  C(13)  C(12)  C(17)  C(16)  AND 
CONT  C(14)  C(18)  C(15)  C(12)  AND 
CONT  C(14)  C(15)  C(12)  C(18)  AND 
CONT  C(14)  C(12)  C(18)  C(15) 
END                                                                             
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_cod_data_source_file            c9dt02449b2.cif
_cod_data_source_block           (L1)H2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        5204.06(15)
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               7701708