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_1514718
_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         'C37 H49.95 Ga Mn N2 O2'
_chemical_formula_sum            'C37 H49.95 Ga Mn N2 O2'
_chemical_formula_weight         679.41
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-05-31
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 103.1581(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1814(2)
_cell_length_b                   20.4882(4)
_cell_length_c                   16.7346(3)
_cell_measurement_reflns_used    7771
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3399.16(11)
_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 0.992
_diffrn_measured_fraction_theta_max 0.989
_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  0.059
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41038
_diffrn_reflns_theta_full        26.904
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         5.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1431.796
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.74
_refine_diff_density_min         -2.07
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0437
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7688
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1473
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.0089359
_refine_ls_shift/su_mean         0.0001445
_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: 
 5.65 6.68 1.85 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2096
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.2096
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                4038
_reflns_number_total             7688
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.98
_oxford_diffrn_Wilson_scale      70.55
_oxford_refine_ls_r_factor_ref   0.1473
_oxford_refine_ls_scale          0.12814(7)
_oxford_reflns_number_all        7688
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 076jtnp12
_cod_data_source_file            c3sc52133h.txt
_cod_data_source_block           global
_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 21/n '
_cod_database_code               1514718
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S U'S 
REM GA(1,U'S) UNTIL C(43) GA(101,U[ISO]) 
RIDE GA(1,U'S) GA(101,U'S) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE GA  (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 123,X'S) H   ( 122,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  20,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   ( 223,X'S) H   ( 222,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 243,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 253,X'S) H   ( 252,X'S) 
RIDE C   (  27,X'S) H   ( 272,X'S) H   ( 271,X'S) H   ( 273,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 342,X'S) H   ( 341,X'S) H   ( 343,X'S) 
RIDE C   (  35,X'S) H   ( 352,X'S) H   ( 351,X'S) H   ( 353,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  40,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) H   ( 423,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 433,X'S) H   ( 432,X'S) H   ( 431,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
PLANAR N(13) N(30) GA(101) MN(2) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;