Adaptive behavior of a redox-active gallium carbenoid in complexes with molybdenum
Igor L. Fedushkin; Vladimir G. Sokolov; Alexander V. Piskunov; Valentine M. Makarov; Eugeny V. Baranov; Gleb A. Abakumov; Chem.Commun. 50 (2014) 10108–; doi:10.1039/C4cc04019H

data_7115529
_publ_section_title
;
 Adaptive behavior of a redox-active gallium carbenoid in complexes with
 molybdenum
;
_journal_name_full               Chem.Commun.
_journal_page_first              10108
_journal_paper_doi               10.1039/C4cc04019H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C44 H45 Ga Mo N2 O3'
_chemical_formula_weight         815.48
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 97.2432(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.82154(13)
_cell_length_b                   38.0697(5)
_cell_length_c                   11.69917(16)
_cell_measurement_reflns_used    23311
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.3423
_cell_measurement_theta_min      3.1267
_cell_volume                     3897.62(9)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            88721
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.414
_diffrn_reflns_theta_min         3.133
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SCALE3 ABSPACK, CrysAlisPro, Agilent Technologies (2012) 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       prism
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 8521 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.009(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1120
_refine_ls_number_reflns         25974
_refine_ls_number_restraints     317
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+1.7939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                21017
_reflns_number_total             25974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc04019h2.cif
_cod_data_source_block           gabianmocpco
_cod_database_code               7115529
_shelx_estimated_absorpt_t_min   0.678
_shelx_estimated_absorpt_t_max   0.858
_shelxl_version_number           2013-4
_shelx_res_checksum              80285