Multiple metal-bound oligomers from Ir-catalysed dehydropolymerisation of H3B·NH3 as probed by experiment and computation
Kumar, Amit; Johnson, Heather C.; Hooper, Thomas N.; Weller, Andrew S.; Algarra, Andrés G.; Macgregor, Stuart A.; Chemical Science 5 (2014) 2546–; doi:10.1039/c4sc00735b

data_1516552
_publ_section_title
;
 Multiple metal-bound oligomers from Ir-catalysed dehydropolymerisation of
 H3B&#x00B7;NH3 as probed by experiment and computation
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              2546
_journal_paper_doi               10.1039/c4sc00735b
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety
'C36 H74 B Ir N P2, C24 H12 B Cl8, C3.80 H2.54 F1.27, C6 H4 F2'
_chemical_formula_sum            'C69.8 H92.54 B2 Cl8 F3.27 Ir N P2'
_chemical_formula_weight         1567.19
_chemical_name_systematic        '[Ir(PCy3)2(H)2(AB)][BArCl4]'
_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             13-11-08
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 105.9144(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.21990(10)
_cell_length_b                   34.9437(2)
_cell_length_c                   18.45950(10)
_cell_measurement_reflns_used    18793
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     8200.57(9)
_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 0.990
_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  0.041
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            118540
_diffrn_reflns_theta_full        26.919
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_min         5.097
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.971
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3203.088
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         1.82
_refine_diff_density_min         -1.21
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0845
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         18580
_refine_ls_number_restraints     1027
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.0159015
_refine_ls_shift/su_mean         0.0005970
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +46.59P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1389
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1389
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              45
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                17148
_reflns_number_total             18580
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.27
_oxford_diffrn_Wilson_scale      42.17
_oxford_refine_ls_r_factor_ref   0.0613
_oxford_refine_ls_scale          0.15675(5)
_oxford_reflns_number_all        18580
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '002ak13 in P2(1)/c'
_cod_data_source_file            c4sc00735b2.cif
_cod_data_source_block           6a
_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/current/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C69.80 H92.54 B2 Cl8 F3.27 Ir1 N1 P2'
_cod_database_code               1516552
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H   (  32,X'S) 
RIDE C   (   4,X'S) H   (  42,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  52,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (   9,X'S) H   (  92,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  12,X'S) H   ( 122,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 172,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 212,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 262,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 272,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 282,X'S) 
RIDE C   (  29,X'S) H   ( 292,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 302,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 332,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 342,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) H   ( 352,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  60,X'S) H   ( 601,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   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) 
RIDE C   (  95,X'S) H   ( 951,X'S) 
RIDE IR  (   1,X'S) H   (   2,X'S) H   (   1,X'S) 
RIDE B   (   1,X'S) H   (   5,X'S) H   (   4,X'S) H   (   3,X'S) 
RIDE N   (   1,X'S) H   (   7,X'S) H   (   8,X'S) H   (   6,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
SAME C(90) C(91) C(92) C(93) C(94) C(95) AND 
CONT C(91) C(92) C(93) C(94) C(95) C(90) AND 
CONT C(92) C(93) C(94) C(95) C(90) C(91) AND 
CONT C(93) C(94) C(95) C(90) C(91) C(92) AND 
CONT C(94) C(95) C(90) C(91) C(92) C(93) AND 
CONT C(95) C(90) C(91) C(92) C(93) C(94) 
SAME F(1) C(92) C(91) C(90) F(3) AND 
CONT F(3) C(90) C(91) C(92) F(1) 
SAME F(1) C(92) C(93) C(94) C(95) C(90) F(3) AND 
CONT F(3) C(90) C(95) C(94) C(93) C(92) F(1) 
SAME F(1) C(92) C(91) C(90) C(95) AND 
CONT F(1) C(92) C(93) C(94) C(95) 
SAME F(3) C(90) C(91) C(92) C(93) AND 
CONT F(3) C(90) C(95) C(94) C(93) 
DELU 0.015 C(90) C(91) C(92) C(93) C(94) C(95) F(3) AND 
CONT C(91) C(92) C(93) C(94) C(95) C(90) F(3) AND 
CONT C(92) C(93) C(94) C(95) C(90) C(91) F(3) AND 
CONT C(93) C(94) C(95) C(90) C(91) C(92) F(3) AND 
CONT C(94) C(95) C(90) C(91) C(92) C(93) F(3) AND 
CONT C(95) C(90) C(91) C(92) C(93) C(04) F(3) 
SIMU 0.015 C(90) C(91) C(92) C(93) C(94) C(95) F(3) AND 
CONT C(91) C(92) C(93) C(94) C(95) C(90) F(3) AND 
CONT C(92) C(93) C(94) C(95) C(90) C(91) F(3) AND 
CONT C(93) C(94) C(95) C(90) C(91) C(92) F(3) AND 
CONT C(94) C(95) C(90) C(91) C(92) C(93) F(3) AND 
CONT C(95) C(90) C(91) C(92) C(93) C(04) F(3) 
DELU 0.015 C(90) C(91) C(92) C(93) C(94) C(95) F(2) AND 
CONT C(91) C(92) C(93) C(94) C(95) C(90) F(2) AND 
CONT C(92) C(93) C(94) C(95) C(90) C(91) F(2) AND 
CONT C(93) C(94) C(95) C(90) C(91) C(92) F(2) AND 
CONT C(94) C(95) C(90) C(91) C(92) C(93) F(2) AND 
CONT C(95) C(90) C(91) C(92) C(93) C(04) F(2) 
SIMU 0.015 C(90) C(91) C(92) C(93) C(94) C(95) F(2) AND 
CONT C(91) C(92) C(93) C(94) C(95) C(90) F(2) AND 
CONT C(92) C(93) C(94) C(95) C(90) C(91) F(2) AND 
CONT C(93) C(94) C(95) C(90) C(91) C(92) F(2) AND 
CONT C(94) C(95) C(90) C(91) C(92) C(93) F(2) AND 
CONT C(95) C(90) C(91) C(92) C(93) C(04) F(2) 
DELU 0.015 C(90) C(91) C(92) C(93) C(94) C(95) F(1) AND 
CONT C(91) C(92) C(93) C(94) C(95) C(90) F(1) AND 
CONT C(92) C(93) C(94) C(95) C(90) C(91) F(1) AND 
CONT C(93) C(94) C(95) C(90) C(91) C(92) F(1) AND 
CONT C(94) C(95) C(90) C(91) C(92) C(93) F(1) AND 
CONT C(95) C(90) C(91) C(92) C(93) C(04) F(1) 
SIMU 0.015 C(90) C(91) C(92) C(93) C(94) C(95) F(1) AND 
CONT C(91) C(92) C(93) C(94) C(95) C(90) F(1) AND 
CONT C(92) C(93) C(94) C(95) C(90) C(91) F(1) AND 
CONT C(93) C(94) C(95) C(90) C(91) C(92) F(1) AND 
CONT C(94) C(95) C(90) C(91) C(92) C(93) F(1) AND 
CONT C(95) C(90) C(91) C(92) C(93) C(04) F(1) 
PLANAR 0.010000  F(1) F(2) F(3) C(90) C(91) C(92) C(93) C(94) C(95) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;