Chemical vapour deposition (CVD) of nickel oxide using the novel nickel dialkylaminoalkoxide precursor [Ni(dmamp′)2] (dmamp′ = 2-dimethylamino-2-methyl-1-propanolate)
Wilson, Rachel L.; Macdonald, Thomas J.; Lin, Chieh-Ting; Xu, Shengda; Taylor, Alaric; Knapp, Caroline E.; Guldin, Stefan; McLachlan, Martyn A.; Carmalt, Claire J.; Blackman, Chris S.; RSC Advances 11 (2021) 22199–22205; doi:10.1039/D1RA03263A

data_7243106
_publ_section_title
;
 Chemical vapour deposition (CVD) of nickel oxide using the novel nickel
 dialkylaminoalkoxide precursor [Ni(dmamp&#x2032;)2] (dmamp&#x2032; =
 2-dimethylamino-2-methyl-1-propanolate)
;
_journal_issue                   36
_journal_name_full               'RSC Advances'
_journal_page_first              22199
_journal_page_last               22205
_journal_paper_doi               10.1039/D1RA03263A
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C12 H28 N2 Ni O2'
_chemical_formula_sum            'C12 H28 N2 Ni O2'
_chemical_formula_weight         291.07
_chemical_name_systematic        'Nickel bisdimetylaminopropanoto'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-17 deposited with the CCDC.	2021-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.29170(10)
_cell_length_b                   10.68490(10)
_cell_length_c                   17.7929(2)
_cell_measurement_reflns_used    11656
_cell_measurement_temperature    150.5(7)
_cell_measurement_theta_max      74.1190
_cell_measurement_theta_min      7.8320
_cell_volume                     1386.26(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.5(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -41.00 -14.00   1.00    1.00    --  -42.62 -57.00  30.00   27
  2  \w    -60.00 -26.00   1.00    1.00    --  -42.62 -38.00 120.00   34
  3  \w    -71.00 -10.00   1.00    1.00    --  -42.62 -77.00 120.00   61
  4  \w    -85.00 -58.00   1.00    1.00    --  -42.62 -57.00  30.00   27
  5  \w   -111.00 -10.00   1.00    1.00    --  -42.62 -77.00 -60.00  101
  6  \w    -43.00 -18.00   1.00    1.00    --  -42.62 -38.00-120.00   25
  7  \w    -69.00 -10.00   1.00    1.00    --  -42.62 -77.00-150.00   59
  8  \w      1.00  63.00   1.00    1.00    --   42.62 -99.00-120.00   62
  9  \w     36.00 136.00   1.00    1.88    --  107.94 -61.00 -30.00  100
 10  \w     78.00 104.00   1.00    1.88    --  107.94 -95.00  30.00   26
 11  \w     26.00 106.00   1.00    1.88    --  107.94 -95.00 -60.00   80
 12  \w     35.00 114.00   1.00    1.88    --  107.94-125.00-180.00   79
 13  \w     34.00 106.00   1.00    1.88    --  107.94 -95.00-150.00   72
 14  \w     24.00  84.00   1.00    1.00    --   42.62-125.00  30.00   60
 15  \w      1.00  57.00   1.00    1.00    --   42.62 -99.00 150.00   56
 16  \w     79.00 105.00   1.00    1.88    --  107.94  61.00 120.00   26
 17  \w     77.00 172.00   1.00    1.88    --  107.94  74.00 170.25   95
 18  \w    132.00 173.00   1.00    1.88    --  107.94  77.00  30.00   41
 19  \w    147.00 176.00   1.00    1.88    --  107.94  61.00 -60.00   29
 20  \w    153.00 178.00   1.00    1.88    --  107.94  61.00-120.00   25
 21  \w     79.00 164.00   1.00    1.88    --  107.94  61.00 -90.00   85
 22  \w     79.00 106.00   1.00    1.88    --  107.94  61.00-120.00   27
 23  \w     79.00 173.00   1.00    1.88    --  107.94  61.00-141.85   94
 24  \w     79.00 105.00   1.00    1.88    --  107.94  61.00   0.00   26
 25  \w     80.00 105.00   1.00    1.88    --  107.94  61.00  30.00   25
 26  \w     79.00 128.00   1.00    1.88    --  107.94  61.00  60.00   49
 27  \w     75.00 176.00   1.00    1.88    --  107.94  77.00   0.00  101
 28  \w     82.00 109.00   1.00    1.88    --  107.94  61.00 -60.00   27
 29  \w     75.00 101.00   1.00    1.88    --  107.94  77.00 -90.00   26
 30  \w     76.00 157.00   1.00    1.88    --  107.94  73.00 -36.61   81
 31  \w     78.00 105.00   1.00    1.88    --  107.94  77.00-180.00   27
 32  \w     75.00 101.00   1.00    1.88    --  107.94  77.00-150.00   26
 33  \w     75.00 101.00   1.00    1.88    --  107.94  77.00-120.00   26
 34  \w     75.00 126.00   1.00    1.88    --  107.94  77.00 -60.00   51
 35  \w     79.00 105.00   1.00    1.88    --  107.94  62.00  11.05   26
 36  \w     75.00 101.00   1.00    1.88    --  107.94  77.00  30.00   26
 37  \w     75.00 102.00   1.00    1.88    --  107.94  77.00  60.00   27
 38  \w     79.00 139.00   1.00    1.88    --  107.94  61.00  90.00   60
 39  \w     80.00 178.00   1.00    1.88    --  107.94  62.00 105.87   98
 40  \w     79.00 114.00   1.00    1.88    --  107.94  61.00 150.00   35
 41  \w     76.00 140.00   1.00    1.88    --  107.94  77.00 150.00   64
 42  \w     76.00 102.00   1.00    1.88    --  107.94  77.00 120.00   26
 43  \w     76.00 101.00   1.00    1.88    --  107.94  77.00 -30.00   25
 44  \w    -65.00  31.00   1.00    1.00    --  -42.62  38.00  60.00   96
 45  \w   -106.00 -61.00   1.00    1.00    --  -42.62 -38.00-120.00   45
 46  \w   -118.00 -10.00   1.00    1.00    --  -42.62 -77.00  30.00  108
 47  \w   -111.00 -79.00   1.00    1.00    --  -42.62 -38.00 120.00   32
 48  \w   -119.00 -88.00   1.00    1.00    --  -42.62 -77.00 120.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0599122000
_diffrn_orient_matrix_UB_12      -0.0763341000
_diffrn_orient_matrix_UB_13      0.0692205000
_diffrn_orient_matrix_UB_21      0.0842476000
_diffrn_orient_matrix_UB_22      -0.1187191000
_diffrn_orient_matrix_UB_23      -0.0349657000
_diffrn_orient_matrix_UB_31      0.1842223000
_diffrn_orient_matrix_UB_32      0.0295340000
_diffrn_orient_matrix_UB_33      0.0385066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19513
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.487
_diffrn_reflns_theta_min         7.857
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.965
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_preparation
'reaction of nickel chloride with Na salt of DMAP'
_exptl_crystal_recrystallization_method 'crystallised from THF'
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0209
_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^)+(0.0313P)^2^+0.3982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1314
_reflns_number_total             1410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra03263a2.cif
_cod_data_source_block           xstr0754
_cod_database_code               7243106
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ni N2 C12 O2'
_chemical_oxdiff_usercomment     'Ni(dmamp)2 RW15 in THF'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
;
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_original_sample_id xstr0754
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.239
_oxdiff_exptl_absorpt_empirical_full_min 0.879