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_1514721
_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         'C36 H41 Co2 Ga1 N2 O7'
_chemical_formula_sum            'C36 H41 Co2 Ga N2 O7'
_chemical_formula_weight         801.32
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90.0148(16)
_cell_angle_beta                 89.9906(18)
_cell_angle_gamma                90.0029(19)
_cell_formula_units_Z            4
_cell_length_a                   8.8239(2)
_cell_length_b                   19.5134(4)
_cell_length_c                   21.4040(4)
_cell_measurement_reflns_used    23826
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     3685.43(13)
_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 0.996
_diffrn_measured_fraction_theta_max 0.987
_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  0.024
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39477
_diffrn_reflns_theta_full        73.815
_diffrn_reflns_theta_max         76.098
_diffrn_reflns_theta_min         3.065
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.219
_exptl_absorpt_correction_T_max  0.44
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         15117
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.0013116
_refine_ls_shift/su_mean         0.0001126
_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: 
 0.127E+04 0.197E+04 0.107E+04 295. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0745
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0744
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              24
_reflns_limit_k_min              -24
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                13685
_reflns_number_total             15179
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.41
_oxford_diffrn_Wilson_scale      0.12
_oxford_refine_ls_r_factor_ref   0.0339
_oxford_refine_ls_scale          2.921(10)
_oxford_reflns_number_all        15120
_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_cell_volume        3685.43(14)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C36 H41 Co2 Ga1 N2 O7'
_cod_database_code               1514721
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 233,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 303,X'S) H   ( 301,X'S) H   ( 302,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   ( 332,X'S) H   ( 333,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  40,X'S) H   ( 402,X'S) H   ( 403,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) H   ( 413,X'S) H   ( 412,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   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 472,X'S) H   ( 473,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) H   ( 483,X'S) H   ( 482,X'S) 
RIDE C   (  49,X'S) H   ( 492,X'S) H   ( 491,X'S) H   ( 493,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  71,X'S) H   ( 713,X'S) H   ( 711,X'S) H   ( 712,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) H   ( 722,X'S) H   ( 723,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   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  78,X'S) H   ( 783,X'S) H   ( 781,X'S) H   ( 782,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) H   ( 792,X'S) H   ( 793,X'S) 
RIDE C   (  81,X'S) H   ( 812,X'S) H   ( 813,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  87,X'S) H   ( 871,X'S) 
RIDE C   (  88,X'S) H   ( 882,X'S) H   ( 883,X'S) H   ( 881,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) H   ( 893,X'S) H   ( 892,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  91,X'S) H   ( 911,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) 
RIDE C   (  94,X'S) H   ( 941,X'S) 
RIDE C   (  95,X'S) H   ( 952,X'S) H   ( 953,X'S) H   ( 951,X'S) 
RIDE C   (  96,X'S) H   ( 961,X'S) H   ( 963,X'S) H   ( 962,X'S) 
RIDE C   (  97,X'S) H   ( 972,X'S) H   ( 971,X'S) H   ( 973,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;