#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:10:13 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234787 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/94/4349453.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_4349453
loop_
_publ_author_name
'Yoo, Changho'
'Lee, Yunho'
_publ_section_title
;
 Formation of a tetranickel octacarbonyl cluster from the CO2 reaction of
 a zero-valent nickel monocarbonyl species
;
_journal_issue                   6
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              849
_journal_paper_doi               10.1039/C6QI00011H
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C27 H40 N Ni O P2'
_chemical_formula_sum            'C27 H40 N Ni O P2'
_chemical_formula_weight         515.25
_chemical_name_common            (PNP)Ni(CO)
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-12 deposited with the CCDC.
2016-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.239(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7516(15)
_cell_length_b                   9.8103(9)
_cell_length_c                   18.1748(17)
_cell_measurement_reflns_used    32589
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.65
_cell_volume                     2796.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Photon 100 CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32589
_diffrn_reflns_theta_full        25.57
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.9219
_exptl_absorpt_correction_T_min  0.8522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.706
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.331
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.331
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
_refine_ls_wR_factor_ref         0.1892
_reflns_number_gt                4056
_reflns_number_total             5233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00011h2.cif
_cod_data_source_block           n0375a-1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4349453
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.22708(4) 0.17257(5) 0.18565(3) 0.0280(2) Uani 1 1 d .
P1 P 0.31302(6) 0.04153(10) 0.25840(6) 0.0185(3) Uani 1 1 d .
P2 P 0.20023(6) 0.35895(10) 0.11787(6) 0.0186(3) Uani 1 1 d .
N1 N 0.2360(2) 0.3020(3) 0.26827(19) 0.0203(7) Uani 1 1 d .
C9 C 0.1843(2) 0.4192(4) 0.2610(2) 0.0167(8) Uani 1 1 d .
C11 C 0.1016(2) 0.5723(4) 0.1764(2) 0.0227(9) Uani 1 1 d .
H11 H 0.0857 0.6011 0.1272 0.027 Uiso 1 1 calc R
C10 C 0.1581(2) 0.4639(4) 0.1883(2) 0.0190(8) Uani 1 1 d .
C4 C 0.4049(2) 0.1375(4) 0.3909(2) 0.0207(9) Uani 1 1 d .
H4 H 0.4324 0.0512 0.3945 0.025 Uiso 1 1 calc R
C13 C 0.0938(2) 0.5946(4) 0.3052(2) 0.0227(9) Uani 1 1 d .
H13 H 0.0720 0.6388 0.3460 0.027 Uiso 1 1 calc R
C2 C 0.2983(2) 0.2868(4) 0.3264(2) 0.0176(8) Uani 1 1 d .
C14 C 0.1503(2) 0.4873(4) 0.3186(2) 0.0206(9) Uani 1 1 d .
H14 H 0.1661 0.4597 0.3680 0.025 Uiso 1 1 calc R
C12 C 0.0678(3) 0.6399(4) 0.2342(2) 0.0245(9) Uani 1 1 d .
C3 C 0.3419(2) 0.1596(4) 0.3334(2) 0.0179(8) Uani 1 1 d .
C6 C 0.3897(3) 0.3633(4) 0.4343(2) 0.0249(9) Uani 1 1 d .
H6 H 0.4062 0.4345 0.4680 0.030 Uiso 1 1 calc R
C7 C 0.3267(3) 0.3881(4) 0.3772(2) 0.0249(9) Uani 1 1 d .
H7 H 0.3022 0.4765 0.3724 0.030 Uiso 1 1 calc R
C22 C 0.2927(3) 0.4575(5) 0.0893(2) 0.0287(10) Uani 1 1 d .
H22 H 0.3177 0.4052 0.0493 0.034 Uiso 1 1 calc R
C5 C 0.4291(2) 0.2361(4) 0.4432(2) 0.0229(9) Uani 1 1 d .
C19 C 0.4152(3) -0.0260(4) 0.2303(2) 0.0264(10) Uani 1 1 d .
H19 H 0.4488 -0.0645 0.2749 0.032 Uiso 1 1 calc R
C25 C 0.1216(3) 0.3638(5) 0.0361(2) 0.0253(9) Uani 1 1 d .
H25 H 0.1149 0.4605 0.0191 0.030 Uiso 1 1 calc R
C8 C 0.4977(3) 0.2108(5) 0.5056(3) 0.0319(11) Uani 1 1 d .
H8A H 0.4712 0.1998 0.5520 0.048 Uiso 1 1 calc R
H8B H 0.5370 0.2884 0.5098 0.048 Uiso 1 1 calc R
H8C H 0.5292 0.1277 0.4955 0.048 Uiso 1 1 calc R
C24 C 0.3605(3) 0.4675(5) 0.1549(3) 0.0368(12) Uani 1 1 d .
H24A H 0.4090 0.5206 0.1406 0.055 Uiso 1 1 calc R
H24B H 0.3797 0.3757 0.1699 0.055 Uiso 1 1 calc R
H24C H 0.3362 0.5125 0.1963 0.055 Uiso 1 1 calc R
C15 C 0.0043(3) 0.7539(5) 0.2208(3) 0.0340(11) Uani 1 1 d .
H15A H 0.0106 0.7953 0.1725 0.051 Uiso 1 1 calc R
H15B H 0.0146 0.8230 0.2595 0.051 Uiso 1 1 calc R
H15C H -0.0536 0.7177 0.2215 0.051 Uiso 1 1 calc R
C16 C 0.2590(3) -0.1046(4) 0.2975(2) 0.0246(9) Uani 1 1 d .
H16 H 0.2388 -0.1656 0.2554 0.029 Uiso 1 1 calc R
C27 C 0.0345(3) 0.3107(5) 0.0542(3) 0.0370(12) Uani 1 1 d .
H27A H -0.0040 0.3056 0.0087 0.056 Uiso 1 1 calc R
H27B H 0.0105 0.3728 0.0891 0.056 Uiso 1 1 calc R
H27C H 0.0411 0.2198 0.0763 0.056 Uiso 1 1 calc R
C18 C 0.3149(3) -0.1908(5) 0.3529(3) 0.0390(12) Uani 1 1 d .
H18A H 0.3348 -0.1347 0.3956 0.059 Uiso 1 1 calc R
H18B H 0.3641 -0.2254 0.3293 0.059 Uiso 1 1 calc R
H18C H 0.2816 -0.2677 0.3693 0.059 Uiso 1 1 calc R
C23 C 0.2673(3) 0.5982(5) 0.0588(3) 0.0397(12) Uani 1 1 d .
H23A H 0.2421 0.6513 0.0969 0.060 Uiso 1 1 calc R
H23B H 0.2257 0.5880 0.0157 0.060 Uiso 1 1 calc R
H23C H 0.3180 0.6454 0.0441 0.060 Uiso 1 1 calc R
C17 C 0.1802(3) -0.0537(5) 0.3319(3) 0.0349(11) Uani 1 1 d .
H17A H 0.1501 -0.1312 0.3515 0.052 Uiso 1 1 calc R
H17B H 0.1423 -0.0070 0.2943 0.052 Uiso 1 1 calc R
H17C H 0.1974 0.0099 0.3721 0.052 Uiso 1 1 calc R
C26 C 0.1553(3) 0.2800(5) -0.0258(2) 0.0388(12) Uani 1 1 d .
H26A H 0.1546 0.1831 -0.0128 0.058 Uiso 1 1 calc R
H26B H 0.2138 0.3081 -0.0324 0.058 Uiso 1 1 calc R
H26C H 0.1191 0.2951 -0.0718 0.058 Uiso 1 1 calc R
C20 C 0.3988(3) -0.1385(5) 0.1736(3) 0.0431(13) Uani 1 1 d .
H20A H 0.3698 -0.1005 0.1282 0.065 Uiso 1 1 calc R
H20B H 0.3627 -0.2087 0.1932 0.065 Uiso 1 1 calc R
H20C H 0.4531 -0.1790 0.1628 0.065 Uiso 1 1 calc R
C21 C 0.4662(3) 0.0896(5) 0.1995(3) 0.0406(12) Uani 1 1 d .
H21A H 0.5220 0.0551 0.1882 0.061 Uiso 1 1 calc R
H21B H 0.4742 0.1628 0.2361 0.061 Uiso 1 1 calc R
H21C H 0.4353 0.1250 0.1543 0.061 Uiso 1 1 calc R
C1 C 0.1678(5) 0.0399(6) 0.1337(4) 0.0627(18) Uani 1 1 d .
O1 O 0.1410(4) -0.0476(5) 0.0996(3) 0.0858(16) Uani 1 1 d .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 Ni1 N1 149.3(3)
C1 Ni1 P1 98.72(19)
N1 Ni1 P1 85.50(10)
C1 Ni1 P2 103.80(18)
N1 Ni1 P2 83.61(10)
P1 Ni1 P2 152.00(5)
C3 P1 C16 107.43(19)
C3 P1 C19 105.66(19)
C16 P1 C19 105.73(19)
C3 P1 Ni1 100.13(13)
C16 P1 Ni1 113.79(13)
C19 P1 Ni1 122.78(15)
C10 P2 C25 106.95(19)
C10 P2 C22 104.36(19)
C25 P2 C22 104.3(2)
C10 P2 Ni1 97.98(13)
C25 P2 Ni1 123.15(15)
C22 P2 Ni1 117.86(15)
C2 N1 C9 121.6(3)
C2 N1 Ni1 120.8(3)
C9 N1 Ni1 117.1(3)
C14 C9 N1 125.5(4)
C14 C9 C10 117.0(4)
N1 C9 C10 117.2(3)
C12 C11 C10 122.1(4)
C11 C10 C9 120.6(4)
C11 C10 P2 126.5(3)
C9 C10 P2 112.8(3)
C5 C4 C3 122.7(4)
C14 C13 C12 122.4(4)
N1 C2 C7 126.0(4)
N1 C2 C3 117.7(3)
C7 C2 C3 116.1(4)
C13 C14 C9 121.3(4)
C11 C12 C13 116.6(4)
C11 C12 C15 121.8(4)
C13 C12 C15 121.6(4)
C4 C3 C2 120.6(4)
C4 C3 P1 125.3(3)
C2 C3 P1 114.0(3)
C7 C6 C5 121.5(4)
C6 C7 C2 122.1(4)
C23 C22 C24 111.5(4)
C23 C22 P2 112.7(3)
C24 C22 P2 108.9(3)
C4 C5 C6 116.9(4)
C4 C5 C8 122.2(4)
C6 C5 C8 120.8(4)
C20 C19 C21 110.7(4)
C20 C19 P1 110.4(3)
C21 C19 P1 109.6(3)
C26 C25 C27 110.7(4)
C26 C25 P2 109.0(3)
C27 C25 P2 111.5(3)
C17 C16 C18 110.6(4)
C17 C16 P1 109.0(3)
C18 C16 P1 115.2(3)
O1 C1 Ni1 171.3(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ni1 C1 1.815(7)
Ni1 N1 1.962(3)
Ni1 P1 2.2151(11)
Ni1 P2 2.2236(12)
P1 C3 1.815(4)
P1 C16 1.842(4)
P1 C19 1.854(4)
P2 C10 1.815(4)
P2 C25 1.846(4)
P2 C22 1.861(4)
N1 C2 1.384(5)
N1 C9 1.408(5)
C9 C14 1.389(5)
C9 C10 1.416(5)
C11 C12 1.389(6)
C11 C10 1.391(5)
C4 C5 1.385(6)
C4 C3 1.391(5)
C13 C14 1.385(6)
C13 C12 1.391(6)
C2 C7 1.401(6)
C2 C3 1.425(5)
C12 C15 1.505(6)
C6 C7 1.390(6)
C6 C5 1.398(6)
C22 C23 1.527(6)
C22 C24 1.529(6)
C5 C8 1.514(6)
C19 C20 1.516(6)
C19 C21 1.526(6)
C25 C26 1.526(6)
C25 C27 1.531(6)
C16 C17 1.525(6)
C16 C18 1.531(6)
C1 O1 1.119(7)
