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_1514725
_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         'C65 H53 B1 Co1 F24 Ga1 N2 O4'
_chemical_formula_sum            'C65 H53 B Co F24 Ga N2 O4'
_chemical_formula_weight         1521.56
_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
_audit_creation_date             13-07-28
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                78.4857(19)
_cell_angle_beta                 83.9447(17)
_cell_angle_gamma                83.4912(18)
_cell_formula_units_Z            2
_cell_length_a                   12.5663(2)
_cell_length_b                   13.2686(3)
_cell_length_c                   20.7262(4)
_cell_measurement_reflns_used    17796
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     3352.25(12)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13907
_diffrn_reflns_theta_full        74.139
_diffrn_reflns_theta_max         76.432
_diffrn_reflns_theta_min         3.415
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.462
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.060
_platon_squeeze_details
;
;
_refine_diff_density_max         1.74
_refine_diff_density_min         -1.09
_refine_ls_extinction_coef       10.177
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9839
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         13849
_refine_ls_number_restraints     486
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.0005839
_refine_ls_shift/su_mean         0.0000194
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 4.47P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1228
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1228
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                12839
_reflns_number_total             13907
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.49
_oxford_diffrn_Wilson_scale      0.12
_oxford_refine_ls_r_factor_ref   0.0521
_oxford_refine_ls_scale          3.24(3)
_oxford_reflns_number_all        13849
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title '079JART13 in P -1'
_cod_data_source_file            c3sc52133h.txt
_cod_data_source_block           079jart13
_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 -1 '
_cod_original_formula_sum        'C65 H53 B1 Co1 F24 Ga1 N2 O4'
_cod_database_code               1514725
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 203,X'S) H   ( 202,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 213,X'S) H   ( 212,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 232,X'S) H   ( 231,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 243,X'S) H   ( 242,X'S) H   ( 241,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 323,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 333,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 393,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) H   ( 403,X'S) H   ( 402,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) H   ( 422,X'S) H   ( 423,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   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  88,X'S) H   ( 881,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  92,X'S) H   ( 921,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME  C(78)  F(1)  F(2)  F(3) AND 
CONT  C(78)  F(2)  F(3)  F(1) AND 
CONT  C(78)  F(3)  F(1)  F(2) AND 
CONT  C(78)  F(51)  F(52)  F(53) AND 
CONT  C(78)  F(52)  F(53)  F(51) AND 
CONT  C(78)  F(53)  F(51)  F(52) 
SIMU 0.01 C(78)  F(1)  F(2)  F(3) AND 
CONT  C(78)  F(2)  F(3)  F(1) AND 
CONT  C(78)  F(3)  F(1)  F(2) AND 
CONT  C(78)  F(51)  F(52)  F(53) AND 
CONT  C(78)  F(52)  F(53)  F(51) AND 
CONT  C(78)  F(53)  F(51)  F(52) 
DELU 0.01 C(78)  F(1)  F(2)  F(3) AND 
CONT  C(78)  F(2)  F(3)  F(1) AND 
CONT  C(78)  F(3)  F(1)  F(2) AND 
CONT  C(78)  F(51)  F(52)  F(53) AND 
CONT  C(78)  F(52)  F(53)  F(51) AND 
CONT  C(78)  F(53)  F(51)  F(52) 
SAME  C(99)  F(4)  F(5)  F(6) AND 
CONT  C(99)  F(5)  F(6)  F(4) AND 
CONT  C(99)  F(6)  F(4)  F(5) AND 
CONT  C(98)  F(54)  F(55)  F(56) AND 
CONT  C(98)  F(55)  F(56)  F(54) AND 
CONT  C(98)  F(56)  F(54)  F(55) 
SIMU 0.01 C(99)  F(4)  F(5)  F(6) AND 
CONT  C(99)  F(5)  F(6)  F(4) AND 
CONT  C(99)  F(6)  F(4)  F(5) AND 
CONT  C(98)  F(54)  F(55)  F(56) AND 
CONT  C(98)  F(55)  F(56)  F(54) AND 
CONT  C(98)  F(56)  F(54)  F(55) 
DELU 0.01 C(99)  F(4)  F(5)  F(6) AND 
CONT  C(99)  F(5)  F(6)  F(4) AND 
CONT  C(99)  F(6)  F(4)  F(5) AND 
CONT  C(98)  F(54)  F(55)  F(56) AND 
CONT  C(98)  F(55)  F(56)  F(54) AND 
CONT  C(98)  F(56)  F(54)  F(55) 
SAME  C(93)  F(7)  F(8)  F(9) AND 
CONT  C(93)  F(8)  F(9)  F(7) AND 
CONT  C(93)  F(9)  F(7)  F(8) AND 
CONT  C(93)  F(57)  F(58)  F(59) AND 
CONT  C(93)  F(58)  F(59)  F(57) AND 
CONT  C(93)  F(59)  F(57)  F(58) 
SIMU 0.01 C(93)  F(7)  F(8)  F(9) AND 
CONT  C(93)  F(8)  F(9)  F(7) AND 
CONT  C(93)  F(9)  F(7)  F(8) AND 
CONT  C(93)  F(57)  F(58)  F(59) AND 
CONT  C(93)  F(58)  F(59)  F(57) AND 
CONT  C(93)  F(59)  F(57)  F(58) 
DELU 0.01 C(93)  F(7)  F(8)  F(9) AND 
CONT  C(93)  F(8)  F(9)  F(7) AND 
CONT  C(93)  F(9)  F(7)  F(8) AND 
CONT  C(93)  F(57)  F(58)  F(59) AND 
CONT  C(93)  F(58)  F(59)  F(57) AND 
CONT  C(93)  F(59)  F(57)  F(58) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;