Second-generation hexavalent molybdenum oxo-amidinate precursors for atomic layer deposition.
Jurca, T.; Peters, A. W.; Mouat, A. R.; Farha, O. K.; Hupp, J. T.; Lohr, T. L.; Delferro, M.; Marks, T. J.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1172–1178; doi:10.1039/c6dt03952a

data_7041549
_publ_section_title
;
 Second-generation hexavalent molybdenum oxo-amidinate precursors for
 atomic layer deposition.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1172
_journal_page_last               1178
_journal_paper_doi               10.1039/c6dt03952a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C28 H50 Mo N4 O2'
_chemical_formula_sum            'C28 H50 Mo N4 O2'
_chemical_formula_weight         570.66
_chemical_name_systematic
'MoO2(R-AMD)2 (AMD = N,N?-di-R-acetamidinate) R = cyclohexyl '
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_audit_update_record
;
2016-10-13 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4715(2)
_cell_length_b                   11.6621(2)
_cell_length_c                   21.5619(5)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.85
_cell_measurement_theta_min      2.66
_cell_volume                     2884.59(10)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.06
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            44589
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         38.211
_diffrn_reflns_theta_min         2.664
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.7475
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0676 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.8852.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.085
_refine_diff_density_max         2.095
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 4398 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.790
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         15363
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.790
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1336
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                11565
_reflns_number_total             15363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03952a2.cif
_cod_data_source_block           sol2
_cod_depositor_comments
'Adding full bibliography for 7041548--7041549.cif.'
_cod_database_code               7041549
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.900
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C17(H17), C3(H3), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B), C11(H11A,H11B), C14(H14A,H14B), C12(H12A,
 H12B), C8(H8A,H8B), C21(H21A,H21B), C18(H18A,H18B), C22(H22A,H22B), C4(H4A,
 H4B), C27(H27A,H27B), C5(H5A,H5B), C28(H28A,H28B), C25(H25A,H25B), C6(H6A,H6B),
  C7(H7A,H7B), C20(H20A,H20B), C19(H19A,H19B), C24(H24A,H24B), C26(H26A,H26B)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C16(H16A,H16B,H16C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_completion    2016-01-11
_olex2_date_sample_data_collection 2016-01-10
_olex2_date_sample_submission    2016-01-10
_olex2_exptl_crystal_mounting_method
'Mounted on a brass tip in Paratone-N under air free conditions.'
_olex2_submission_original_sample_id TJ109
_olex2_submission_special_instructions 'No special instructions were received'