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_7041548
_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         'C16 H34 Mo N4 O2'
_chemical_formula_sum            'C16 H34 Mo N4 O2'
_chemical_formula_weight         410.41
_chemical_name_systematic
'MoO2(R-AMD)2 (AMD = N,N?-di-R-acetamidinate) R = isopropyl'
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-08-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_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                   10.3994(4)
_cell_length_b                   10.3994(4)
_cell_length_c                   18.7146(9)
_cell_measurement_reflns_used    9673
_cell_measurement_temperature    100
_cell_measurement_theta_max      53.30
_cell_measurement_theta_min      2.98
_cell_volume                     2023.94(15)
_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)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            71443
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         54.817
_diffrn_reflns_theta_min         2.976
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0960 before and 0.0607 after correction.
The Ratio of minimum to maximum transmission is 0.8958.
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    1.347
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.348
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 4250 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         12623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.0090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                10832
_reflns_number_total             12623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03952a2.cif
_cod_data_source_block           tj129_a
_cod_depositor_comments
'Adding full bibliography for 7041548--7041549.cif.'
_cod_original_cell_volume        2023.94(18)
_cod_database_code               7041548
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.768
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Mo1A)=0.5*(1-FVAR(2))
 Sof(Mo1)=0.5*FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C)
;
_shelx_res_checksum              6146
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-02-06
_olex2_date_sample_submission    2016-02-06
_olex2_exptl_crystal_mounting_method 'Mounted at 100 K on a brass tip.'
_olex2_submission_original_sample_id TJ129
_olex2_submission_special_instructions 'No special instructions were received'