#------------------------------------------------------------------------------
#$Date: 2017-02-23 07:05:07 +0200 (Thu, 23 Feb 2017) $
#$Revision: 192475 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/22/7042207.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_7042207
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            'C38 H42 N4 Ni O2'
_chemical_formula_weight         645.46
_chemical_name_common            NioPP2Py3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.031(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5179(5)
_cell_length_b                   14.6472(8)
_cell_length_c                   15.7614(8)
_cell_measurement_reflns_used    368
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      29.6972
_cell_measurement_theta_min      1.9220
_cell_volume                     2122.13(19)
_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)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Apex II Bruker 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  0.0343
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25626
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.93
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '  SADABS-2014/5 (Bruker,201)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.627
_exptl_crystal_size_mid          0.308
_exptl_crystal_size_min          0.256
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.407
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0426
_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)+(0.0536P)²+2.5316P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                3093
_reflns_number_total             3878
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04083g2.cif
_cod_data_source_block           I
_cod_database_code               7042207
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.5 0.5 0.01890(14) Uani d . P S 1
N N1 0.6700(2) 0.48648(14) 0.43253(13) 0.0234(5) Uani d . . . 1
O O1 0.55242(18) 0.63389(11) 0.53039(11) 0.0236(4) Uani d . . . 1
N N2 0.3364(2) 0.53131(14) 0.38264(13) 0.0227(4) Uani d . . . 1
C C1 0.5575(2) 0.71157(17) 0.49001(16) 0.0226(5) Uani d . . . 1
C C6 0.5872(3) 0.79429(18) 0.53878(17) 0.0295(6) Uani d . . . 1
C C15 0.2535(3) 0.60553(17) 0.37773(17) 0.0259(6) Uani d . . . 1
H H15 0.2635 0.6416 0.4291 0.031 Uiso calc U . R 1
C C2 0.5352(3) 0.71822(19) 0.39796(16) 0.0269(6) Uani d . . . 1
H H2 0.5199 0.6641 0.3635 0.032 Uiso calc U . R 1
C C14 0.7746(3) 0.54929(19) 0.44460(17) 0.0287(6) Uani d . . . 1
H H14 0.7707 0.5995 0.482 0.034 Uiso calc U . R 1
C C3 0.5354(3) 0.8018(2) 0.35693(18) 0.0355(7) Uani d . . . 1
H H3 0.5193 0.8041 0.2949 0.043 Uiso calc U . R 1
C C16 0.1537(3) 0.6325(2) 0.30161(19) 0.0354(7) Uani d . . . 1
H H16 0.0968 0.686 0.3007 0.043 Uiso calc U . R 1
C C4 0.5584(3) 0.8816(2) 0.4047(2) 0.0400(7) Uani d . . . 1
H H4 0.5562 0.9389 0.3761 0.048 Uiso calc U . R 1
C C5 0.5848(3) 0.87665(19) 0.4950(2) 0.0371(7) Uani d . . . 1
H H5 0.6019 0.9315 0.5283 0.044 Uiso calc U . R 1
C C19 0.3183(3) 0.4809(2) 0.31015(17) 0.0347(7) Uani d . . . 1
H H19 0.3754 0.4273 0.3128 0.042 Uiso calc U . R 1
C C10 0.6793(3) 0.4156(2) 0.3812(2) 0.0377(7) Uani d . . . 1
H H10 0.6074 0.3692 0.3734 0.045 Uiso calc U . R 1
C C13 0.8883(3) 0.5450(2) 0.4054(2) 0.0394(7) Uani d . . . 1
H H13 0.9604 0.5914 0.4157 0.047 Uiso calc U . R 1
C C17 0.1382(3) 0.5803(2) 0.22702(19) 0.0473(8) Uani d . . . 1
H H17 0.0717 0.5977 0.1734 0.057 Uiso calc U . R 1
C C18 0.2207(4) 0.5028(2) 0.23160(19) 0.0491(9) Uani d . . . 1
H H18 0.2108 0.4648 0.1815 0.059 Uiso calc U . R 1
C C7 0.6269(4) 0.7893(2) 0.6383(2) 0.0499(9) Uani d . . . 1
H H7 0.5646 0.7416 0.6557 0.06 Uiso calc U . R 1
C C12 0.8959(4) 0.4725(2) 0.3514(2) 0.0520(9) Uani d . . . 1
H H12 0.9728 0.468 0.3234 0.062 Uiso calc U . R 1
C C11 0.7893(4) 0.4067(2) 0.3388(3) 0.0579(10) Uani d . . . 1
H H11 0.7911 0.3558 0.3017 0.069 Uiso calc U . R 1
C C9 0.7907(4) 0.7579(4) 0.6719(3) 0.0858(16) Uani d . . . 1
H H9A 0.8068 0.704 0.6388 0.129 Uiso calc U . R 1
H H9B 0.8123 0.7428 0.7345 0.129 Uiso calc U . R 1
H H9C 0.8547 0.8075 0.6632 0.129 Uiso calc U . R 1
C C8 0.6125(8) 0.8749(3) 0.6865(3) 0.117(2) Uani d . . . 1
H H8A 0.6753 0.9222 0.672 0.176 Uiso calc U . R 1
H H8B 0.6416 0.8632 0.7499 0.176 Uiso calc U . R 1
H H8C 0.5112 0.8956 0.6694 0.176 Uiso calc U . R 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 3_666 . 180.0
O1 Ni1 N2 3_666 . 85.67(7)
O1 Ni1 N2 . . 94.33(7)
O1 Ni1 N2 3_666 3_666 94.33(7)
O1 Ni1 N2 . 3_666 85.67(7)
N2 Ni1 N2 . 3_666 180.00(11)
O1 Ni1 N1 3_666 3_666 91.99(7)
O1 Ni1 N1 . 3_666 88.01(7)
N2 Ni1 N1 . 3_666 86.32(7)
N2 Ni1 N1 3_666 3_666 93.67(7)
O1 Ni1 N1 3_666 . 88.01(7)
O1 Ni1 N1 . . 91.99(7)
N2 Ni1 N1 . . 93.67(7)
N2 Ni1 N1 3_666 . 86.33(7)
N1 Ni1 N1 3_666 . 180.0
C10 N1 C14 . . 117.3(2)
C10 N1 Ni1 . . 123.07(17)
C14 N1 Ni1 . . 119.55(17)
C1 O1 Ni1 . . 138.99(16)
C19 N2 C15 . . 117.3(2)
C19 N2 Ni1 . . 121.76(17)
C15 N2 Ni1 . . 120.85(17)
O1 C1 C2 . . 122.9(2)
O1 C1 C6 . . 120.3(2)
C2 C1 C6 . . 116.8(2)
C5 C6 C1 . . 119.8(2)
C5 C6 C7 . . 121.6(3)
C1 C6 C7 . . 118.6(2)
N2 C15 C16 . . 123.2(3)
N2 C15 H15 . . 118.4
C16 C15 H15 . . 118.4
C3 C2 C1 . . 121.5(3)
C3 C2 H2 . . 119.3
C1 C2 H2 . . 119.3
N1 C14 C13 . . 123.3(3)
N1 C14 H14 . . 118.4
C13 C14 H14 . . 118.4
C4 C3 C2 . . 121.0(3)
C4 C3 H3 . . 119.5
C2 C3 H3 . . 119.5
C17 C16 C15 . . 118.7(3)
C17 C16 H16 . . 120.7
C15 C16 H16 . . 120.7
C3 C4 C5 . . 118.6(3)
C3 C4 H4 . . 120.7
C5 C4 H4 . . 120.7
C4 C5 C6 . . 122.2(3)
C4 C5 H5 . . 118.9
C6 C5 H5 . . 118.9
N2 C19 C18 . . 123.2(3)
N2 C19 H19 . . 118.4
C18 C19 H19 . . 118.4
N1 C10 C11 . . 122.9(3)
N1 C10 H10 . . 118.5
C11 C10 H10 . . 118.5
C12 C13 C14 . . 119.1(3)
C12 C13 H13 . . 120.5
C14 C13 H13 . . 120.5
C18 C17 C16 . . 118.8(3)
C18 C17 H17 . . 120.6
C16 C17 H17 . . 120.6
C17 C18 C19 . . 118.8(3)
C17 C18 H18 . . 120.6
C19 C18 H18 . . 120.6
C8 C7 C6 . . 117.1(3)
C8 C7 C9 . . 106.7(4)
C6 C7 C9 . . 108.7(3)
C8 C7 H7 . . 108.0
C6 C7 H7 . . 108.0
C9 C7 H7 . . 108.0
C13 C12 C11 . . 118.4(3)
C13 C12 H12 . . 120.8
C11 C12 H12 . . 120.8
C12 C11 C10 . . 119.0(3)
C12 C11 H11 . . 120.5
C10 C11 H11 . . 120.5
C7 C9 H9A . . 109.5
C7 C9 H9B . . 109.5
H9A C9 H9B . . 109.5
C7 C9 H9C . . 109.5
H9A C9 H9C . . 109.5
H9B C9 H9C . . 109.5
C7 C8 H8A . . 109.5
C7 C8 H8B . . 109.5
H8A C8 H8B . . 109.5
C7 C8 H8C . . 109.5
H8A C8 H8C . . 109.5
H8B C8 H8C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ni1 O1 3_666 2.0494(17)
Ni1 O1 . 2.0494(17)
Ni1 N2 . 2.136(2)
Ni1 N2 3_666 2.136(2)
Ni1 N1 3_666 2.1634(19)
Ni1 N1 . 2.1634(19)
N1 C10 . 1.332(3)
N1 C14 . 1.333(3)
O1 C1 . 1.311(3)
N2 C19 . 1.333(3)
N2 C15 . 1.334(3)
C1 C2 . 1.414(3)
C1 C6 . 1.423(4)
C6 C5 . 1.387(4)
C6 C7 . 1.517(4)
C15 C16 . 1.381(4)
C15 H15 . 0.95
C2 C3 . 1.384(4)
C2 H2 . 0.95
C14 C13 . 1.379(4)
C14 H14 . 0.95
C3 C4 . 1.377(4)
C3 H3 . 0.95
C16 C17 . 1.378(4)
C16 H16 . 0.95
C4 C5 . 1.383(4)
C4 H4 . 0.95
C5 H5 . 0.95
C19 C18 . 1.379(4)
C19 H19 . 0.95
C10 C11 . 1.387(4)
C10 H10 . 0.95
C13 C12 . 1.374(5)
C13 H13 . 0.95
C17 C18 . 1.372(4)
C17 H17 . 0.95
C18 H18 . 0.95
C7 C8 . 1.491(5)
C7 C9 . 1.579(6)
C7 H7 . 1.0
C12 C11 . 1.376(5)
C12 H12 . 0.95
C11 H11 . 0.95
C9 H9A . 0.98
C9 H9B . 0.98
C9 H9C . 0.98
C8 H8A . 0.98
C8 H8B . 0.98
C8 H8C . 0.98
