Coordination chemistry of phosphinocarbynes: phosphorus vs. carbyne site selectivity.
Colebatch, Annie L.; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4355–4365; doi:10.1039/c6dt04770j

data_7042313
_publ_section_title
;
 Coordination chemistry of phosphinocarbynes: phosphorus vs. carbyne site
 selectivity.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4355
_journal_page_last               4365
_journal_paper_doi               10.1039/c6dt04770j
_journal_volume                  46
_journal_year                    2017
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C42 H49 Au3 B2 Cl3 N12 O4 P1 W2, C H2 Cl2'
_chemical_formula_sum            'C43 H51 Au3 B2 Cl5 N12 O4 P W2'
_chemical_formula_weight         1988.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2016-11-20 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.0601(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.7948(4)
_cell_length_b                   10.6312(2)
_cell_length_c                   24.9238(5)
_cell_measurement_reflns_used    101682
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.55
_cell_volume                     5663.91(19)
_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    'Ortep-3 for Windows v. 2.01'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.136
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            68238
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.570
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.105
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.329
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         4.16
_refine_diff_density_min         -3.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9445
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9972
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.0009430
_refine_ls_shift/su_mean         0.0000359
_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: 
 21.0 31.3 16.1 4.32 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1602
_refine_ls_wR_factor_gt          0.1340
_refine_ls_wR_factor_ref         0.1602
_reflns_limit_h_max              25
_reflns_limit_h_min              -28
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                7173
_reflns_number_total             9980
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.06
_oxford_diffrn_Wilson_scale      418.75
_oxford_refine_ls_r_factor_ref   0.0865
_oxford_refine_ls_scale          0.050516(9)
_oxford_reflns_number_all        9972
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c6dt04770j1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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.

'_atom_sites_solution_primary' value 'Direct' changed to 'direct'
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 7042309--7042314.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C43 H51 Au3 B2 Cl5 N12 O4 P1 W2'
_cod_database_code               7042313
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) H   ( 253,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) H   ( 313,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) H   ( 353,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 412,X'S) H   ( 413,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) H   ( 452,X'S) H   ( 453,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) H   ( 513,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) H   ( 552,X'S) H   ( 553,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) H   ( 612,X'S) H   ( 613,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) H   ( 652,X'S) H   ( 653,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) H   (1002,X'S) 
RIDE B   (  1,X'S)  H   ( 11,X'S) 
RIDE B   (  2,X'S)  H   ( 21,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
DIST 1.37 , 0.01 = C(71) TO C(76) 
DIST 1.37 , 0.01 = C(75) TO C(76) 
REM 
U(IJ) 0.0 , 0.005 = C(71) TO C(76) 
U(IJ) 0.0 , 0.005 = C(75) TO C(76) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;