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_1514724
_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 H48 Ga1 Mn1 N2 O2'
_chemical_formula_sum            'C37 H48 Ga Mn N2 O2'
_chemical_formula_weight         677.45
_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             13-07-01
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90.0077(7)
_cell_angle_beta                 90.0065(7)
_cell_angle_gamma                85.7423(5)
_cell_formula_units_Z            4
_cell_length_a                   8.83270(10)
_cell_length_b                   18.3781(2)
_cell_length_c                   20.6752(2)
_cell_measurement_reflns_used    13419
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3346.91(6)
_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 0.989
_diffrn_measured_fraction_theta_max 0.985
_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  0.023
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            89054
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_min         5.137
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.74
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9366
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         15175
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.0009050
_refine_ls_shift/su_mean         0.0000419
_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: 
 19.9 28.6 13.9 3.51 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0919
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0919
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                11421
_reflns_number_total             15175
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.88
_oxford_diffrn_Wilson_scale      9.67
_oxford_refine_ls_r_factor_ref   0.0560
_oxford_refine_ls_scale          0.32307(16)
_oxford_reflns_number_all        15175
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title '077jart13 in P -1'
_cod_data_source_file            c3sc52133h.txt
_cod_data_source_block           077jart13
_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        'C37 H48 Ga1 Mn1 N2 O2'
_cod_database_code               1514724
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIV PART(1001,OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
WEIGHT -1 PART(2002,OCC) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (   4,X'S) H   (  42,X'S) H   (  41,X'S) H   (  43,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 303,X'S) H   ( 302,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) 
RIDE C   (  39,X'S) H   ( 393,X'S) H   ( 392,X'S) H   ( 391,X'S) 
RIDE C   (  44,X'S) H   ( 443,X'S) H   ( 442,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 453,X'S) H   ( 452,X'S) H   ( 451,X'S) 
RIDE C   (  28,X'S) H   ( 281,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   (  52,X'S) H   ( 521,X'S) H   ( 523,X'S) H   ( 522,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) 
RIDE C   (  42,X'S) H   ( 423,X'S) H   ( 422,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 433,X'S) H   ( 432,X'S) H   ( 431,X'S) 
RIDE C   (  53,X'S) H   ( 533,X'S) H   ( 532,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  57,X'S) H   ( 572,X'S) H   ( 571,X'S) H   ( 573,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  65,X'S) H   ( 651,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) H   ( 663,X'S) H   ( 662,X'S) 
RIDE C   (  71,X'S) H   ( 711,X'S) H   ( 713,X'S) H   ( 712,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  68,X'S) H   ( 683,X'S) H   ( 682,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 693,X'S) H   ( 692,X'S) H   ( 691,X'S) 
RIDE C   (  75,X'S) H   ( 753,X'S) H   ( 752,X'S) H   ( 751,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  89,X'S) H   ( 891,X'S) 
RIDE C   (  90,X'S) H   ( 901,X'S) 
RIDE C   (  91,X'S) H   ( 911,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  73,X'S) H   (  72,X'S) 
RIDE C   (  83,X'S) H   ( 831,X'S) H   ( 833,X'S) H   ( 832,X'S) 
RIDE C   (  93,X'S) H   ( 931,X'S) 
RIDE C   (  94,X'S) H   ( 943,X'S) H   ( 942,X'S) H   ( 941,X'S) 
RIDE C   (  86,X'S) H   ( 863,X'S) H   ( 862,X'S) H   ( 861,X'S) 
RIDE C   (  95,X'S) H   ( 953,X'S) H   ( 952,X'S) H   ( 951,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
SAME  GA(2)  N(14)  N(30) AND 
CONT  GA(2)  N(30)  N(14) AND 
CONT  GA(3)  N(82)  N(58) AND 
CONT  GA(3)  N(58)  N(82) 
SIMU 0.01  GA(2)  MN(2) AND 
CONT  GA(3)  MN(46) 
DELU 0.01  GA(2)  MN(2) AND 
CONT  GA(3)  MN(46) 
END                                                                             
;