#------------------------------------------------------------------------------
#$Date: 2023-10-13 02:02:11 +0300 (Fri, 13 Oct 2023) $
#$Revision: 286938 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/41/7714185.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_7714185
loop_
_publ_author_name
'Moussa, Mehdi'
'Rummel, Eva-Maria'
'Eckhardt, Maria'
'Riesinger, Christoph'
'Scheer, Manfred'
_publ_section_title
;
 Unusual cleavage of phosphaalkynes triple bond in the coordination sphere
 of transition metals
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02472E
_journal_year                    2023
_chemical_formula_moiety         'C19 H3 Co6 O17 P'
_chemical_formula_sum            'C19 H3 Co6 O17 P'
_chemical_formula_weight         887.76
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-03-01
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.01.27 svn.rdd5efbe3 for OlexSys, GUI svn.r6708)
;
_audit_update_record
;
2023-07-16 deposited with the CCDC.	2023-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.715(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1777(2)
_cell_length_b                   14.2641(2)
_cell_length_c                   16.3093(2)
_cell_measurement_reflns_used    4587
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      34.984
_cell_measurement_theta_min      4.451
_cell_volume                     2683.20(7)
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'Oxford Diffraction, Gemini R Ultra'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22840
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.984
_diffrn_reflns_theta_min         2.324
_exptl_absorpt_coefficient_mu    3.763
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.198
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_recrystallization_method
'The material was recrystallised from n-hexane by by cooling to +5 degrees'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         10854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0239P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7790
_reflns_number_total             10854
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02472e2.cif
_cod_data_source_block           em34
_cod_database_code               7714185
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.453
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Instruments CryoJet'
_olex2_submission_special_instructions 'No special instructions were received'
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_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.05656(13) 0.57860(12) 0.37629(11) 0.0224(3) Uani 1 1 d . . . . .
C2 C 0.04489(13) 0.76874(11) 0.37189(11) 0.0226(3) Uani 1 1 d . . . . .
C3 C -0.10589(13) 0.66991(11) 0.23434(10) 0.0204(3) Uani 1 1 d . . . . .
C4 C 0.22941(15) 0.77532(11) 0.14068(11) 0.0246(3) Uani 1 1 d . . . . .
C5 C 0.12862(13) 0.87250(11) 0.24192(11) 0.0207(3) Uani 1 1 d . . . . .
C6 C -0.01147(14) 0.77054(11) 0.09924(11) 0.0230(3) Uani 1 1 d . . . . .
C7 C 0.22813(13) 0.56121(10) 0.13912(10) 0.0183(3) Uani 1 1 d . . . . .
C8 C 0.14310(12) 0.47186(11) 0.25191(10) 0.0184(3) Uani 1 1 d . . . . .
C9 C -0.01349(13) 0.56250(11) 0.10691(11) 0.0220(3) Uani 1 1 d . . . . .
C10 C 0.45164(11) 0.57429(10) 0.33357(9) 0.0156(3) Uani 1 1 d . . . . .
C11 C 0.37878(12) 0.60356(10) 0.47763(10) 0.0169(3) Uani 1 1 d . . . . .
C12 C 0.36626(12) 0.79737(10) 0.42842(10) 0.0164(3) Uani 1 1 d . . . . .
C13 C 0.53280(12) 0.67286(11) 0.22364(10) 0.0197(3) Uani 1 1 d . . . . .
C14 C 0.69980(12) 0.60835(11) 0.37417(10) 0.0190(3) Uani 1 1 d . . . . .
C15 C 0.63711(13) 0.80104(11) 0.34963(11) 0.0211(3) Uani 1 1 d . . . . .
C16 C 0.58713(13) 0.89235(11) 0.48930(11) 0.0197(3) Uani 1 1 d . . . . .
C17 C 0.43674(13) 0.90281(11) 0.31700(11) 0.0205(3) Uani 1 1 d . . . . .
C18 C 0.56072(12) 0.69985(10) 0.45434(10) 0.0150(3) Uani 1 1 d . . . . .
C19 C 0.63683(12) 0.67307(10) 0.54292(10) 0.0196(3) Uani 1 1 d . . . . .
H19A H 0.604381 0.698263 0.586118 0.029 Uiso 1 1 calc R U . . .
H19B H 0.714684 0.698802 0.553019 0.029 Uiso 1 1 calc R U . . .
H19C H 0.641345 0.604599 0.547706 0.029 Uiso 1 1 calc R U . . .
Co1 Co 0.04746(2) 0.67264(2) 0.30050(2) 0.01449(4) Uani 1 1 d . . . . .
Co2 Co 0.12076(2) 0.75970(2) 0.19195(2) 0.01490(4) Uani 1 1 d . . . . .
Co3 Co 0.12353(2) 0.58167(2) 0.19500(2) 0.01373(4) Uani 1 1 d . . . . .
Co4 Co 0.40022(2) 0.67458(2) 0.39515(2) 0.01224(4) Uani 1 1 d . . . . .
Co5 Co 0.56770(2) 0.67346(2) 0.34107(2) 0.01427(4) Uani 1 1 d . . . . .
Co6 Co 0.51454(2) 0.81832(2) 0.39942(2) 0.01518(4) Uani 1 1 d . . . . .
O1 O 0.06353(11) 0.51980(9) 0.42449(9) 0.0380(3) Uani 1 1 d . . . . .
O2 O 0.03957(11) 0.82779(9) 0.41708(9) 0.0359(3) Uani 1 1 d . . . . .
O3 O -0.20133(10) 0.66927(8) 0.19516(9) 0.0316(3) Uani 1 1 d . . . . .
O4 O 0.29917(12) 0.78430(10) 0.10939(10) 0.0439(4) Uani 1 1 d . . . . .
O5 O 0.13325(10) 0.94435(8) 0.27354(8) 0.0294(3) Uani 1 1 d . . . . .
O6 O -0.08979(11) 0.77723(10) 0.03910(8) 0.0373(3) Uani 1 1 d . . . . .
O7 O 0.29525(10) 0.54816(8) 0.10621(8) 0.0270(3) Uani 1 1 d . . . . .
O8 O 0.15456(10) 0.40289(8) 0.28861(8) 0.0269(3) Uani 1 1 d . . . . .
O9 O -0.09612(10) 0.55039(9) 0.05116(8) 0.0346(3) Uani 1 1 d . . . . .
O10 O 0.42732(9) 0.49926(7) 0.30720(7) 0.0210(2) Uani 1 1 d . . . . .
O11 O 0.36665(11) 0.55639(8) 0.52982(8) 0.0310(3) Uani 1 1 d . . . . .
O12 O 0.30202(9) 0.84232(7) 0.45047(8) 0.0229(2) Uani 1 1 d . . . . .
O13 O 0.51393(10) 0.67097(9) 0.15107(8) 0.0310(3) Uani 1 1 d . . . . .
O14 O 0.78550(9) 0.56924(8) 0.39356(8) 0.0286(3) Uani 1 1 d . . . . .
O15 O 0.71271(11) 0.83789(8) 0.33382(9) 0.0336(3) Uani 1 1 d . . . . .
O16 O 0.63276(10) 0.94053(8) 0.54467(8) 0.0287(3) Uani 1 1 d . . . . .
O17 O 0.38498(10) 0.95471(9) 0.26796(9) 0.0336(3) Uani 1 1 d . . . . .
P1 P 0.22604(3) 0.67284(2) 0.29869(2) 0.01235(7) 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'
Co Co 0.3494 0.9721 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 Co1 179.21(16) . . ?
O2 C2 Co1 177.44(15) . . ?
O3 C3 Co1 178.23(15) . . ?
O4 C4 Co2 178.86(17) . . ?
O5 C5 Co2 179.77(18) . . ?
O6 C6 Co2 176.39(16) . . ?
O7 C7 Co3 178.34(14) . . ?
O8 C8 Co3 179.01(14) . . ?
O9 C9 Co3 178.10(16) . . ?
Co4 C10 Co5 77.63(5) . . ?
O10 C10 Co4 141.23(12) . . ?
O10 C10 Co5 141.14(12) . . ?
O11 C11 Co4 178.25(14) . . ?
Co4 C12 Co6 77.28(5) . . ?
O12 C12 Co4 145.55(12) . . ?
O12 C12 Co6 137.15(12) . . ?
O13 C13 Co5 178.01(14) . . ?
O14 C14 Co5 177.43(15) . . ?
Co6 C15 Co5 77.18(6) . . ?
O15 C15 Co5 138.44(13) . . ?
O15 C15 Co6 144.34(13) . . ?
O16 C16 Co6 178.49(14) . . ?
O17 C17 Co6 176.85(14) . . ?
C19 C18 Co4 130.92(11) . . ?
C19 C18 Co5 132.62(11) . . ?
C19 C18 Co6 132.63(11) . . ?
Co5 C18 Co4 80.26(6) . . ?
Co6 C18 Co4 80.26(5) . . ?
Co6 C18 Co5 79.58(6) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C1 Co1 C2 97.62(7) . . ?
C1 Co1 C3 102.39(7) . . ?
C1 Co1 Co2 151.76(5) . . ?
C1 Co1 Co3 97.36(5) . . ?
C1 Co1 P1 99.66(5) . . ?
C2 Co1 C3 99.82(7) . . ?
C2 Co1 Co2 99.24(5) . . ?
C2 Co1 Co3 154.86(5) . . ?
C2 Co1 P1 103.36(5) . . ?
C3 Co1 Co2 96.85(5) . . ?
C3 Co1 Co3 96.53(5) . . ?
C3 Co1 P1 145.36(5) . . ?
Co2 Co1 Co3 59.722(8) . . ?
P1 Co1 Co2 54.375(11) . . ?
P1 Co1 Co3 54.114(11) . . ?
C4 Co2 C5 99.26(7) . . ?
C4 Co2 C6 100.95(8) . . ?
C4 Co2 Co1 149.44(5) . . ?
C4 Co2 Co3 97.26(5) . . ?
C4 Co2 P1 96.31(5) . . ?
C5 Co2 C6 101.81(7) . . ?
C5 Co2 Co1 95.80(5) . . ?
C5 Co2 Co3 152.90(5) . . ?
C5 Co2 P1 102.39(5) . . ?
C6 Co2 Co1 101.77(5) . . ?
C6 Co2 Co3 95.94(5) . . ?
C6 Co2 P1 147.44(5) . . ?
Co3 Co2 Co1 60.288(8) . . ?
P1 Co2 Co1 54.328(11) . . ?
P1 Co2 Co3 54.336(11) . . ?
C7 Co3 C9 101.02(7) . . ?
C7 Co3 Co1 152.37(5) . . ?
C7 Co3 Co2 99.10(5) . . ?
C7 Co3 P1 99.57(5) . . ?
C8 Co3 C7 96.97(7) . . ?
C8 Co3 C9 102.16(7) . . ?
C8 Co3 Co1 96.40(5) . . ?
C8 Co3 Co2 151.67(5) . . ?
C8 Co3 P1 99.86(5) . . ?
C9 Co3 Co1 99.64(5) . . ?
C9 Co3 Co2 97.48(5) . . ?
C9 Co3 P1 147.60(5) . . ?
Co2 Co3 Co1 59.991(8) . . ?
P1 Co3 Co1 54.249(11) . . ?
P1 Co3 Co2 54.521(11) . . ?
C10 Co4 Co5 51.43(4) . . ?
C10 Co4 Co6 110.52(4) . . ?
C10 Co4 P1 91.06(4) . . ?
C11 Co4 C10 96.94(6) . . ?
C11 Co4 C12 102.12(6) . . ?
C11 Co4 C18 95.75(7) . . ?
C11 Co4 Co5 127.48(5) . . ?
C11 Co4 Co6 132.39(5) . . ?
C11 Co4 P1 101.17(5) . . ?
C12 Co4 C10 160.72(6) . . ?
C12 Co4 Co5 112.65(4) . . ?
C12 Co4 Co6 53.40(4) . . ?
C12 Co4 P1 88.09(4) . . ?
C18 Co4 C10 87.34(6) . . ?
C18 Co4 C12 87.90(6) . . ?
C18 Co4 Co5 49.83(4) . . ?
C18 Co4 Co6 49.77(4) . . ?
C18 Co4 P1 163.07(5) . . ?
Co6 Co4 Co5 59.465(8) . . ?
P1 Co4 Co5 117.541(13) . . ?
P1 Co4 Co6 115.836(13) . . ?
C10 Co5 C15 159.61(6) . . ?
C10 Co5 Co4 50.95(4) . . ?
C10 Co5 Co6 110.81(4) . . ?
C13 Co5 C10 90.61(6) . . ?
C13 Co5 C15 91.63(7) . . ?
C13 Co5 C18 161.27(6) . . ?
C13 Co5 Co4 115.75(5) . . ?
C13 Co5 Co6 114.25(5) . . ?
C14 Co5 C10 101.75(6) . . ?
C14 Co5 C13 101.48(7) . . ?
C14 Co5 C15 97.65(6) . . ?
C14 Co5 C18 97.20(7) . . ?
C14 Co5 Co4 131.55(5) . . ?
C14 Co5 Co6 130.32(5) . . ?
C15 Co5 Co4 110.46(5) . . ?
C15 Co5 Co6 50.27(5) . . ?
C18 Co5 C10 87.03(6) . . ?
C18 Co5 C15 84.37(6) . . ?
C18 Co5 Co4 49.91(4) . . ?
C18 Co5 Co6 50.16(4) . . ?
Co6 Co5 Co4 60.233(8) . . ?
C12 Co6 Co4 49.32(4) . . ?
C12 Co6 Co5 109.41(4) . . ?
C15 Co6 C12 160.89(6) . . ?
C15 Co6 Co4 112.81(5) . . ?
C15 Co6 Co5 52.55(5) . . ?
C16 Co6 C12 97.95(6) . . ?
C16 Co6 C15 100.03(7) . . ?
C16 Co6 C17 102.49(7) . . ?
C16 Co6 C18 98.27(6) . . ?
C16 Co6 Co4 129.68(5) . . ?
C16 Co6 Co5 133.84(5) . . ?
C17 Co6 C12 88.77(6) . . ?
C17 Co6 C15 93.62(7) . . ?
C17 Co6 C18 158.94(7) . . ?
C17 Co6 Co4 111.88(5) . . ?
C17 Co6 Co5 114.22(5) . . ?
C18 Co6 C12 84.88(6) . . ?
C18 Co6 C15 86.17(6) . . ?
C18 Co6 Co4 49.96(4) . . ?
C18 Co6 Co5 50.26(4) . . ?
Co5 Co6 Co4 60.302(8) . . ?
Co1 P1 Co2 71.297(13) . . ?
Co1 P1 Co4 136.597(19) . . ?
Co2 P1 Co4 138.441(19) . . ?
Co3 P1 Co1 71.637(13) . . ?
Co3 P1 Co2 71.143(13) . . ?
Co3 P1 Co4 137.945(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Co1 1.8034(17) . ?
C1 O1 1.1339(19) . ?
C2 Co1 1.8053(17) . ?
C2 O2 1.1347(19) . ?
C3 Co1 1.8331(15) . ?
C3 O3 1.1325(18) . ?
C4 Co2 1.7916(17) . ?
C4 O4 1.130(2) . ?
C5 Co2 1.7923(16) . ?
C5 O5 1.1405(18) . ?
C6 Co2 1.8278(16) . ?
C6 O6 1.1315(19) . ?
C7 Co3 1.8119(16) . ?
C7 O7 1.1281(18) . ?
C8 Co3 1.7971(16) . ?
C8 O8 1.1367(18) . ?
C9 Co3 1.8397(16) . ?
C9 O9 1.1322(18) . ?
C10 Co4 1.9624(15) . ?
C10 Co5 1.9755(14) . ?
C10 O10 1.1559(17) . ?
C11 Co4 1.7691(16) . ?
C11 O11 1.1312(18) . ?
C12 Co4 1.9176(15) . ?
C12 Co6 2.0301(15) . ?
C12 O12 1.1544(18) . ?
C13 Co5 1.8239(16) . ?
C13 O13 1.1313(19) . ?
C14 Co5 1.7845(15) . ?
C14 O14 1.1352(17) . ?
C15 Co5 1.9925(16) . ?
C15 Co6 1.9303(16) . ?
C15 O15 1.1588(19) . ?
C16 Co6 1.7927(16) . ?
C16 O16 1.1291(18) . ?
C17 Co6 1.8275(16) . ?
C17 O17 1.1232(18) . ?
C18 C19 1.494(2) . ?
C18 Co4 1.9160(14) . ?
C18 Co5 1.9136(15) . ?
C18 Co6 1.9107(14) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
Co1 Co2 2.5469(3) . ?
Co1 Co3 2.5545(3) . ?
Co1 P1 2.1843(4) . ?
Co2 Co3 2.5400(3) . ?
Co2 P1 2.1856(4) . ?
Co3 P1 2.1806(4) . ?
Co4 Co5 2.4682(3) . ?
Co4 Co6 2.4665(3) . ?
Co4 P1 2.1984(4) . ?
Co5 Co6 2.4474(3) . ?
