Rearrangement of bis(alkylidynyl)phosphines to phospha-acyls.
Colebatch, Annie L.; Han, Yong-Shen; Hill, Anthony F.; Sharma, Manab; Shang, Rong; Ward, Jas S.; Chemical communications (Cambridge, England) 53 (2017) 1832–1835; doi:10.1039/c6cc09764b

data_7119241
_publ_section_title
;
 Rearrangement of bis(alkylidynyl)phosphines to phospha-acyls.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1832
_journal_page_last               1835
_journal_paper_doi               10.1039/c6cc09764b
_journal_volume                  53
_journal_year                    2017
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C42 H55 B2 N12 O4 P1 W2, C6 H6'
_chemical_formula_sum            'C48 H61 B2 N12 O4 P W2'
_chemical_formula_weight         1290.39
_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     other
_audit_creation_date             13-12-04
_audit_creation_method           CRYSTALS_ver_14.23
_audit_update_record
;
2016-11-28 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.9841(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2055(3)
_cell_length_b                   10.40920(10)
_cell_length_c                   25.5107(3)
_cell_measurement_reflns_used    172784
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     6179.17(12)
_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      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  0.042
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
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_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14148
_diffrn_reflns_theta_full        27.474
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         2.560
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.792
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_platon_squeeze_details
;
;
_refine_diff_density_max         1.74
_refine_diff_density_min         -2.19
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9504
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         14144
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.0030543
_refine_ls_shift/su_mean         0.0001635
_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: 
 18.3 26.9 13.7 3.67 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0999
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0999
_reflns_limit_h_max              30
_reflns_limit_h_min              -31
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                10493
_reflns_number_total             14148
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.25
_oxford_diffrn_Wilson_scale      127.75
_oxford_refine_ls_r_factor_ref   0.0584
_oxford_refine_ls_scale          0.11172(2)
_oxford_reflns_number_all        14144
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'ALC734 At 9:58 on 28/11'
_cod_data_source_file            c6cc09764b2.cif
_cod_data_source_block           ALC734
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7119239--7119242.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C48 H61 B2 N12 O4 P1 W2'
_cod_database_code               7119241
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 113,X'S) H   ( 112,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  15,X'S) H   ( 153,X'S) H   ( 152,X'S) H   ( 151,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 213,X'S) H   ( 212,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 253,X'S) H   ( 252,X'S) H   ( 251,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   ( 353,X'S) H   ( 352,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   ( 453,X'S) H   ( 452,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   ( 552,X'S) H   ( 551,X'S) H   ( 553,X'S) 
RIDE C   (  61,X'S) H   ( 612,X'S) H   ( 611,X'S) H   ( 613,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  65,X'S) H   ( 652,X'S) H   ( 651,X'S) H   ( 653,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) H   ( 732,X'S) 
RIDE C   (  74,X'S) H   ( 742,X'S) H   ( 741,X'S) 
RIDE C   (  75,X'S) H   ( 752,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) H   ( 762,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) 
RIDE C   (  86,X'S) H   ( 861,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 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;