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_7042309
_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 H51 B1 Cl6 N6 O2 P1 Rh1 W1'
_chemical_formula_sum            'C42 H51 B Cl6 N6 O2 P Rh W'
_chemical_formula_weight         1213.16
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2014-04-07 deposited with the CCDC.
2017-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.9517(2)
_cell_length_b                   21.1340(2)
_cell_length_c                   22.12610(10)
_cell_measurement_reflns_used    123670
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.55
_cell_volume                     9797.29(14)
_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  0.073
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            157502
_diffrn_reflns_theta_full        30.048
_diffrn_reflns_theta_max         30.048
_diffrn_reflns_theta_min         2.666
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.084
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4816
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.25
_refine_diff_density_min         -2.20
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9458
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         14323
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.0039986
_refine_ls_shift/su_mean         0.0000373
_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: 
 57.8 94.7 58.1 25.0 6.13 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1063
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1063
_reflns_limit_h_max              29
_reflns_limit_h_min              0
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                11541
_reflns_number_total             14324
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0549
_oxford_refine_ls_scale          0.11955(3)
_oxford_reflns_number_all        14323
_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 'Orthorhombic' changed to
'orthorhombic' 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 b c a '
_cod_original_formula_sum        'C42 H51 B1 Cl6 N6 O2 P1 Rh1 W1'
_cod_database_code               7042309
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 143,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 153,X'S) H   ( 152,X'S) H   ( 151,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 241,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 252,X'S) H   ( 251,X'S) H   ( 253,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 343,X'S) H   ( 342,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 353,X'S) H   ( 352,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 663,X'S) H   ( 662,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) H   ( 673,X'S) H   ( 672,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) H   ( 683,X'S) H   ( 682,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) H   ( 693,X'S) H   ( 692,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) H   ( 703,X'S) H   ( 702,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) H   ( 712,X'S) 
RIDE C   (  72,X'S) H   ( 722,X'S) H   ( 721,X'S) 
RIDE B   (   1,X'S) H   (  11,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                                                                             
;