#------------------------------------------------------------------------------
#$Date: 2017-02-23 07:05:07 +0200 (Thu, 23 Feb 2017) $
#$Revision: 192475 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/22/7042209.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7042209
loop_
_publ_author_name
'Treadwell, LaRico J.'
'Boyle, Timothy J.'
'Phelan, W. Adam'
'Parkes, Marie V.'
'Young, David P.'
_publ_section_title
;
 Synthesis and characterization of a series of nickel(II) alkoxide
 precursors and their utility for Ni(0) nanoparticle production
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C6DT04083G
_journal_year                    2017
_chemical_formula_sum            'C35 H41 N3 Ni O2'
_chemical_formula_weight         594.42
_chemical_name_common            NioMP2Py
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2016-10-19 deposited with the CCDC.
2017-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.808(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6799(16)
_cell_length_b                   13.4323(16)
_cell_length_c                   19.632(2)
_cell_measurement_reflns_used    2542
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      25.0563
_cell_measurement_theta_min      2.2221
_cell_volume                     3304.3(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker XT Intrinsic Solution Method'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX II CCD '
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2496
_diffrn_reflns_av_unetI/netI     0.2197
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18004
_diffrn_reflns_theta_full        25.28
_diffrn_reflns_theta_max         25.28
_diffrn_reflns_theta_min         2.10
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.781
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.2131
_refine_ls_R_factor_gt           0.0769
_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/[σ²(Fo²)+(0.0961P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.2204
_reflns_number_gt                1254
_reflns_number_total             2984
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04083g2.cif
_cod_data_source_block           I
_cod_database_code               7042209
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
Ni Ni1 0.5 0.43109(10) 0.75 0.0344(5) Uani d T P S 1
O O1 0.6437(3) 0.4298(3) 0.80378(19) 0.0300(11) Uani d . . . 1
N N1 0.5696(4) 0.4491(4) 0.6608(2) 0.0331(15) Uani d . . . 1
N N2 0.5 0.2800(6) 0.75 0.032(2) Uani d T P S 1
C C1 0.6984(6) 0.4978(5) 0.8433(3) 0.0325(18) Uani d . . . 1
C C2 0.6631(6) 0.5961(5) 0.8461(3) 0.0381(19) Uani d . . . 1
H H2 0.5967 0.6141 0.8197 0.046 Uiso calc . . R 1
C C3 0.7211(6) 0.6678(6) 0.8858(3) 0.041(2) Uani d . . . 1
H H3 0.6946 0.7338 0.887 0.049 Uiso calc . . R 1
C C4 0.8179(6) 0.6424(6) 0.9238(4) 0.0413(19) Uani d . . . 1
H H4 0.8596 0.6916 0.9503 0.05 Uiso calc . . R 1
C C5 0.8543(6) 0.5464(6) 0.9233(3) 0.043(2) Uani d . . . 1
H H5 0.9204 0.5308 0.9509 0.051 Uiso calc . . R 1
C C6 0.7994(6) 0.4704(5) 0.8845(3) 0.0361(18) Uani d . . . 1
C C7 0.8401(6) 0.3642(6) 0.8847(3) 0.0385(19) Uani d . . . 1
C C8 0.9466(6) 0.3513(6) 0.9336(4) 0.071(3) Uani d . . . 1
H H8A 1.0008 0.3944 0.9185 0.107 Uiso calc . . GR 1
H H8B 0.9697 0.2817 0.9328 0.107 Uiso calc . . GR 1
H H8C 0.9368 0.3695 0.9806 0.107 Uiso calc . . GR 1
C C9 0.8636(6) 0.3358(6) 0.8120(4) 0.052(2) Uani d . . . 1
H H9A 0.802 0.3529 0.7774 0.078 Uiso calc . . GR 1
H H9B 0.8772 0.264 0.8102 0.078 Uiso calc . . GR 1
H H9C 0.9265 0.3723 0.8022 0.078 Uiso calc . . GR 1
C C10 0.7601(6) 0.2921(6) 0.9060(3) 0.051(2) Uani d . . . 1
H H10A 0.7419 0.312 0.9508 0.076 Uiso calc . . GR 1
H H10B 0.7908 0.225 0.9095 0.076 Uiso calc . . GR 1
H H10C 0.6955 0.2923 0.8715 0.076 Uiso calc . . GR 1
C C11 0.6624(6) 0.4949(6) 0.6616(4) 0.041(2) Uani d . . . 1
H H11 0.6956 0.5243 0.7034 0.049 Uiso calc . . R 1
C C12 0.7129(7) 0.5016(6) 0.6039(4) 0.052(2) Uani d . . . 1
H H12 0.7788 0.5359 0.6061 0.062 Uiso calc . . R 1
C C13 0.6658(8) 0.4579(6) 0.5436(4) 0.057(3) Uani d . . . 1
H H13 0.699 0.4608 0.5034 0.068 Uiso calc . . R 1
C C14 0.5705(7) 0.4102(6) 0.5426(3) 0.052(2) Uani d . . . 1
H H14 0.5363 0.3798 0.5013 0.063 Uiso calc . . R 1
C C15 0.5240(6) 0.4061(5) 0.6019(3) 0.042(2) Uani d . . . 1
H H15 0.4581 0.3721 0.6008 0.051 Uiso calc . . R 1
C C16 0.4172(5) 0.2295(5) 0.7662(3) 0.0314(17) Uani d . . . 1
H H16 0.3578 0.2656 0.7775 0.038 Uiso calc . . R 1
C C17 0.4137(6) 0.1273(6) 0.7673(3) 0.043(2) Uani d . . . 1
H H17 0.3539 0.0929 0.7796 0.052 Uiso calc . . R 1
C C18 0.5 0.0766(9) 0.75 0.051(3) Uani d T P S 1
H H18 0.5 0.0058 0.75 0.062 Uiso calc T P RS 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Ni1 O1 2_656 . 179.0(3)
O1 Ni1 N1 2_656 2_656 88.60(19)
O1 Ni1 N1 . 2_656 91.52(19)
O1 Ni1 N1 2_656 . 91.52(18)
O1 Ni1 N1 . . 88.60(19)
O1 Ni1 N2 . . 89.50(14)
O1 Ni1 N2 2_656 . 89.51(14)
N1 Ni1 N1 . 2_656 166.8(3)
N2 Ni1 N1 . . 96.62(16)
N2 Ni1 N1 . 2_656 96.62(16)
C1 O1 Ni1 . . 132.0(4)
C11 N1 Ni1 . . 122.1(4)
C11 N1 C15 . . 118.3(6)
C15 N1 Ni1 . . 119.4(5)
C16 N2 Ni1 . . 120.7(4)
C16 N2 Ni1 2_656 . 120.7(4)
C16 N2 C16 2_656 . 118.6(9)
O1 C1 C2 . . 122.2(7)
O1 C1 C6 . . 119.3(6)
C2 C1 C6 . . 118.5(6)
C1 C2 H2 . . 118.8
C3 C2 C1 . . 122.4(7)
C3 C2 H2 . . 118.8
C2 C3 H3 . . 120.4
C4 C3 C2 . . 119.1(7)
C4 C3 H3 . . 120.4
C3 C4 H4 . . 119.9
C5 C4 C3 . . 120.1(7)
C5 C4 H4 . . 119.9
C4 C5 H5 . . 118.2
C4 C5 C6 . . 123.6(7)
C6 C5 H5 . . 118.2
C1 C6 C7 . . 120.7(6)
C5 C6 C1 . . 116.2(7)
C5 C6 C7 . . 123.1(7)
C6 C7 C8 . . 111.9(6)
C6 C7 C9 . . 110.0(6)
C8 C7 C9 . . 105.8(6)
C10 C7 C6 . . 111.2(6)
C10 C7 C8 . . 108.5(6)
C10 C7 C9 . . 109.2(6)
C7 C8 H8A . . 109.5
C7 C8 H8B . . 109.5
C7 C8 H8C . . 109.5
H8A C8 H8B . . 109.5
H8A C8 H8C . . 109.5
H8B C8 H8C . . 109.5
C7 C9 H9A . . 109.5
C7 C9 H9B . . 109.5
C7 C9 H9C . . 109.5
H9A C9 H9B . . 109.5
H9A C9 H9C . . 109.5
H9B C9 H9C . . 109.5
C7 C10 H10A . . 109.5
C7 C10 H10B . . 109.5
C7 C10 H10C . . 109.5
H10A C10 H10B . . 109.5
H10A C10 H10C . . 109.5
H10B C10 H10C . . 109.5
N1 C11 H11 . . 118.6
N1 C11 C12 . . 122.7(7)
C12 C11 H11 . . 118.6
C11 C12 H12 . . 120.6
C13 C12 C11 . . 118.8(8)
C13 C12 H12 . . 120.6
C12 C13 H13 . . 120.6
C14 C13 C12 . . 118.7(7)
C14 C13 H13 . . 120.6
C13 C14 H14 . . 120.1
C13 C14 C15 . . 119.7(7)
C15 C14 H14 . . 120.1
N1 C15 C14 . . 121.7(7)
N1 C15 H15 . . 119.1
C14 C15 H15 . . 119.1
N2 C16 H16 . . 118.6
N2 C16 C17 . . 122.9(7)
C17 C16 H16 . . 118.6
C16 C17 H17 . . 121.2
C16 C17 C18 . . 117.5(8)
C18 C17 H17 . . 121.2
C17 C18 C17 . 2_656 120.6(11)
C17 C18 H18 . . 119.7
C17 C18 H18 2_656 . 119.7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 O1 2_656 1.961(4)
Ni1 O1 . 1.961(4)
Ni1 N1 . 2.092(5)
Ni1 N1 2_656 2.092(5)
Ni1 N2 . 2.029(8)
O1 C1 . 1.324(7)
N1 C11 . 1.326(8)
N1 C15 . 1.342(8)
N2 C16 . 1.329(7)
N2 C16 2_656 1.329(7)
C1 C2 . 1.397(9)
C1 C6 . 1.453(9)
C2 H2 . 0.95
C2 C3 . 1.378(9)
C3 H3 . 0.95
C3 C4 . 1.378(9)
C4 H4 . 0.95
C4 C5 . 1.370(10)
C5 H5 . 0.95
C5 C6 . 1.394(9)
C6 C7 . 1.517(9)
C7 C8 . 1.541(9)
C7 C9 . 1.551(9)
C7 C10 . 1.508(9)
C8 H8A . 0.98
C8 H8B . 0.98
C8 H8C . 0.98
C9 H9A . 0.98
C9 H9B . 0.98
C9 H9C . 0.98
C10 H10A . 0.98
C10 H10B . 0.98
C10 H10C . 0.98
C11 H11 . 0.95
C11 C12 . 1.387(9)
C12 H12 . 0.95
C12 C13 . 1.373(11)
C13 H13 . 0.95
C13 C14 . 1.366(10)
C14 H14 . 0.95
C14 C15 . 1.385(9)
C15 H15 . 0.95
C16 H16 . 0.95
C16 C17 . 1.373(9)
C17 H17 . 0.95
C17 C18 . 1.375(8)
C18 C17 2_656 1.375(9)
C18 H18 . 0.95
