Formation of sub-valent carbenoid ligands by metal-mediated dehydrogenation chemistry: coordination and activation of H2Ga{(NDippCMe)2CH}
Turner, Joshua; Abdalla, Joseph A. B.; Bates, Joshua I.; Tirfoin, Remi; Kelly, Michael J.; Phillips, Nicholas; Aldridge, Simon; Chemical Science 4 (2013) 4245–; doi:10.1039/c3sc52133h

data_1514720
_publ_section_title
;
 Formation of sub-valent carbenoid ligands by metal-mediated
 dehydrogenation chemistry: coordination and activation of
 H2Ga{(NDippCMe)2CH}
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              4245
_journal_paper_doi               10.1039/c3sc52133h
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety         'C34 H41 Ga1 N2 O5 W1'
_chemical_formula_sum            'C34 H41 Ga N2 O5 W'
_chemical_formula_weight         811.28
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2ab'
_symmetry_space_group_name_H-M   'P b n m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.15777(10)
_cell_length_b                   35.5896(6)
_cell_length_c                   21.1050(3)
_cell_measurement_reflns_used    14158
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     6878.57(17)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37303
_diffrn_reflns_theta_full        74.563
_diffrn_reflns_theta_max         76.084
_diffrn_reflns_theta_min         3.249
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.378
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.62
_refine_diff_density_min         -2.15
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7319
_refine_ls_number_restraints     220
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.0233517
_refine_ls_shift/su_mean         0.0010188
_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: 
 0.208E+04 0.327E+04 0.209E+04 898. 194. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1196
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1196
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              44
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                6867
_reflns_number_total             7351
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.08
_oxford_diffrn_Wilson_scale      1.08
_oxford_refine_ls_r_factor_ref   0.0620
_oxford_refine_ls_scale          0.929(2)
_oxford_reflns_number_all        7319
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c3sc52133h.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 b n m '
_cod_original_formula_sum        'C34 H41 Ga1 N2 O5 W1'
_cod_database_code               1514720
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 122,X'S) H   ( 123,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 143,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) H   ( 183,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) H   ( 372,X'S) H   ( 373,X'S) 
RIDE C   (  38,X'S) H   ( 382,X'S) H   ( 383,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 401,X'S) H   ( 402,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   (  44,X'S) H   ( 442,X'S) H   ( 441,X'S) H   ( 443,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
SAME C(5)  C(13) C(14) C(15) AND 
CONT C(5)  C(13) C(15) C(14) AND 
CONT C(9)  C(10) C(11) C(12) AND 
CONT C(9)  C(10) C(12) C(11) AND 
CONT C(31) C(39) C(40) C(41) AND 
CONT C(31) C(39) C(41) C(40) AND 
CONT C(35) C(36) C(37) C(38) AND 
CONT C(35) C(36) C(38) C(37) 
SIMU 0.01  C(5)  C(13) C(14) C(15) AND 
CONT C(5)  C(13) C(15) C(14) AND 
CONT C(9)  C(10) C(11) C(12) AND 
CONT C(9)  C(10) C(12) C(11) AND 
CONT C(31) C(39) C(40) C(41) AND 
CONT C(31) C(39) C(41) C(40) AND 
CONT C(35) C(36) C(37) C(38) AND 
CONT C(35) C(36) C(38) C(37) 
DELU 0.01  C(5)  C(13) C(14) C(15) AND 
CONT C(5)  C(13) C(15) C(14) AND 
CONT C(9)  C(10) C(11) C(12) AND 
CONT C(9)  C(10) C(12) C(11) AND 
CONT C(31) C(39) C(40) C(41) AND 
CONT C(31) C(39) C(41) C(40) AND 
CONT C(35) C(36) C(37) C(38) AND 
CONT C(35) C(36) C(38) C(37) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;