#------------------------------------------------------------------------------
#$Date: 2021-09-06 14:22:03 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268792 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/78/7707835.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_7707835
loop_
_publ_author_name
'Preißing, Lars'
'Behling, Elias'
'Schnepf, Andreas'
_publ_section_title
;
 GeClₓ[Co(CO)₃PR₃]₄₋ₓ (x =
 0-3; R = ⁿPr, ⁿBu): from cobalt substituted
 germanes to novel binary cluster compounds.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10789
_journal_page_last               10797
_journal_paper_doi               10.1039/d1dt02016a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C12 H21 Cl3 Co Ge O3 P'
_chemical_formula_sum            'C12 H21 Cl3 Co Ge O3 P'
_chemical_formula_weight         482.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-12 deposited with the CCDC.	2021-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.392(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1543(11)
_cell_length_b                   18.346(2)
_cell_length_c                   11.0901(12)
_cell_measurement_reflns_used    5535
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.800
_cell_measurement_theta_min      2.293
_cell_volume                     2065.4(4)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34206
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.510
_diffrn_reflns_theta_min         2.146
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1083 before and 0.0553 after correction. The Ratio of minimum to maximum transmission is 0.7935. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       plank
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.053
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         6300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0382
_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/[σ²(Fo²)+(0.0432P)²+0.8143P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4387
_reflns_number_total             6300
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02016a2.cif
_cod_data_source_block           84
_cod_depositor_comments
'Adding full bibliography for 7707835--7707841.cif.'
_cod_database_code               7707835
_shelx_shelxl_version_number     2014/7
_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   0.869
_shelx_estimated_absorpt_t_min   0.598
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C104(H10H,H10I), C105(H10J,H10K), C106(H10L,
 H10M), C107(H10N,H10O)
2.b Idealised Me refined as rotating group:
 C00K(H00A,H00B,H00C), C103(H10E,H10F,H10G), C108(H10P,H10Q,H10R)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Ge1 Ge 0.32479(2) 0.66755(2) 0.37844(2) 0.02507(8) Uani 1 1 d . . . . .
Co1 Co 0.54921(3) 0.66397(2) 0.38309(3) 0.02144(9) Uani 1 1 d . . . . .
Cl11 Cl 0.22848(7) 0.62706(5) 0.21454(7) 0.04387(19) Uani 1 1 d . . . . .
Cl12 Cl 0.23443(7) 0.77421(4) 0.39666(7) 0.04240(18) Uani 1 1 d . . . . .
Cl13 Cl 0.22569(6) 0.60672(4) 0.51819(6) 0.03773(17) Uani 1 1 d . . . . .
P1 P 0.76732(6) 0.66468(3) 0.38431(5) 0.02035(13) Uani 1 1 d . . . . .
O12 O 0.5283(2) 0.50548(11) 0.35987(19) 0.0434(5) Uani 1 1 d . . . . .
O14 O 0.5413(2) 0.75367(14) 0.1656(2) 0.0541(6) Uani 1 1 d . . . . .
O16 O 0.5368(2) 0.72685(14) 0.62464(19) 0.0531(6) Uani 1 1 d . . . . .
C00K C 0.8838(4) 0.88405(17) 0.3831(3) 0.0502(8) Uani 1 1 d . . . . .
H00A H 0.8522 0.9260 0.3359 0.075 Uiso 1 1 calc GR . . . .
H00B H 0.9751 0.8733 0.3625 0.075 Uiso 1 1 calc GR . . . .
H00C H 0.8796 0.8953 0.4693 0.075 Uiso 1 1 calc GR . . . .
C11 C 0.5391(2) 0.56703(16) 0.3697(2) 0.0294(6) Uani 1 1 d . . . . .
C13 C 0.5449(2) 0.71892(17) 0.2505(3) 0.0343(6) Uani 1 1 d . . . . .
C15 C 0.5439(2) 0.70278(16) 0.5304(3) 0.0323(6) Uani 1 1 d . . . . .
C101 C 0.8379(3) 0.64258(17) 0.2387(3) 0.0358(6) Uani 1 1 d . . . . .
H10A H 0.8172 0.6829 0.1820 0.043 Uiso 1 1 calc R . . . .
H10B H 0.9349 0.6405 0.2493 0.043 Uiso 1 1 calc R . . . .
C102 C 0.7919(3) 0.57212(18) 0.1815(3) 0.0422(7) Uani 1 1 d . . . . .
H10C H 0.6977 0.5766 0.1575 0.051 Uiso 1 1 calc R . . . .
H10D H 0.8001 0.5323 0.2415 0.051 Uiso 1 1 calc R . . . .
C103 C 0.8705(3) 0.55255(19) 0.0717(3) 0.0507(8) Uani 1 1 d . . . . .
H10E H 0.8641 0.5922 0.0127 0.076 Uiso 1 1 calc GR . . . .
H10F H 0.8353 0.5077 0.0356 0.076 Uiso 1 1 calc GR . . . .
H10G H 0.9630 0.5451 0.0959 0.076 Uiso 1 1 calc GR . . . .
C104 C 0.8421(3) 0.75162(15) 0.4250(3) 0.0346(6) Uani 1 1 d . . . . .
H10H H 0.8252 0.7608 0.5113 0.041 Uiso 1 1 calc R . . . .
H10I H 0.9386 0.7468 0.4171 0.041 Uiso 1 1 calc R . . . .
C105 C 0.7979(3) 0.81821(16) 0.3544(3) 0.0429(7) Uani 1 1 d . . . . .
H10J H 0.7055 0.8296 0.3736 0.051 Uiso 1 1 calc R . . . .
H10K H 0.8013 0.8075 0.2670 0.051 Uiso 1 1 calc R . . . .
C106 C 0.8471(3) 0.60034(16) 0.4875(2) 0.0326(6) Uani 1 1 d . . . . .
H10L H 0.8304 0.5505 0.4564 0.039 Uiso 1 1 calc R . . . .
H10M H 0.9433 0.6087 0.4857 0.039 Uiso 1 1 calc R . . . .
C107 C 0.8060(3) 0.60284(17) 0.6171(2) 0.0383(7) Uani 1 1 d . . . . .
H10N H 0.7167 0.5817 0.6230 0.046 Uiso 1 1 calc R . . . .
H10O H 0.8015 0.6543 0.6435 0.046 Uiso 1 1 calc R . . . .
C108 C 0.9002(3) 0.56152(18) 0.7010(3) 0.0445(7) Uani 1 1 d . . . . .
H10P H 0.9065 0.5107 0.6742 0.067 Uiso 1 1 calc GR . . . .
H10Q H 0.8674 0.5630 0.7833 0.067 Uiso 1 1 calc GR . . . .
H10R H 0.9875 0.5842 0.6994 0.067 Uiso 1 1 calc GR . . . .
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'
Cl Cl 0.1484 0.1585 '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'
Ge Ge 0.1547 1.8001 '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
Cl11 Ge1 Co1 116.00(2) . . ?
Cl11 Ge1 Cl13 102.35(3) . . ?
Cl12 Ge1 Co1 116.62(2) . . ?
Cl12 Ge1 Cl11 101.72(3) . . ?
Cl12 Ge1 Cl13 101.07(3) . . ?
Cl13 Ge1 Co1 116.64(2) . . ?
P1 Co1 Ge1 177.80(2) . . ?
C11 Co1 Ge1 88.36(8) . . ?
C11 Co1 P1 93.54(8) . . ?
C13 Co1 Ge1 87.75(8) . . ?
C13 Co1 P1 90.34(8) . . ?
C13 Co1 C11 119.58(13) . . ?
C13 Co1 C15 121.95(14) . . ?
C15 Co1 Ge1 87.54(8) . . ?
C15 Co1 P1 92.54(8) . . ?
C15 Co1 C11 118.06(13) . . ?
C101 P1 Co1 113.99(9) . . ?
C104 P1 Co1 114.70(9) . . ?
C104 P1 C101 104.11(14) . . ?
C104 P1 C106 103.66(13) . . ?
C106 P1 Co1 115.44(9) . . ?
C106 P1 C101 103.51(13) . . ?
O12 C11 Co1 177.7(2) . . ?
O14 C13 Co1 179.4(3) . . ?
O16 C15 Co1 178.0(2) . . ?
C102 C101 P1 116.0(2) . . ?
C101 C102 C103 112.2(3) . . ?
C105 C104 P1 117.6(2) . . ?
C104 C105 C00K 111.9(3) . . ?
C107 C106 P1 116.8(2) . . ?
C106 C107 C108 112.6(3) . . ?
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
Ge1 Co1 2.2791(4) . ?
Ge1 Cl11 2.1739(8) . ?
Ge1 Cl12 2.1726(8) . ?
Ge1 Cl13 2.1763(7) . ?
Co1 P1 2.2146(7) . ?
Co1 C11 1.788(3) . ?
Co1 C13 1.783(3) . ?
Co1 C15 1.784(3) . ?
P1 C101 1.828(3) . ?
P1 C104 1.818(3) . ?
P1 C106 1.820(3) . ?
O12 C11 1.139(3) . ?
O14 C13 1.137(3) . ?
O16 C15 1.139(3) . ?
C00K C105 1.519(4) . ?
C101 C102 1.509(4) . ?
C102 C103 1.515(4) . ?
C104 C105 1.513(4) . ?
C106 C107 1.507(4) . ?
C107 C108 1.521(4) . ?
