#------------------------------------------------------------------------------
#$Date: 2025-04-03 08:32:21 +0300 (Thu, 03 Apr 2025) $
#$Revision: 298703 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/36/7133609.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_7133609
loop_
_publ_author_name
'Samanta, Arup'
'Chaubey, Amit'
'Pal, Debjyoti'
'Majhi, Krishna'
'Srimani, Dipankar'
_publ_section_title
;
 Redox-enabled cooperative catalysis by activating secondary alcohols
 using low-valent Zn complexes.
;
_journal_issue                   75
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10398
_journal_page_last               10401
_journal_paper_doi               10.1039/d4cc03407d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_sum            'C15 H17 Br2 N3 S Zn'
_chemical_formula_weight         496.56
_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   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-05-23 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.335(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5800(18)
_cell_length_b                   12.603(3)
_cell_length_c                   19.172(5)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      23.19
_cell_measurement_theta_min      2.67
_cell_volume                     1830.0(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48694
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.934
_exptl_absorpt_coefficient_mu    5.821
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3209
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0424
_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)+(0.1000P)²+0.8146P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2220
_reflns_number_total             3209
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc03407d2.cif
_cod_data_source_block           AS-Zn-Me_a
_cod_depositor_comments
;
Adding full bibliography for 7133608--7133611.cif.

2025-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C60 H68 Br8 N12 S4 Zn4'
_cod_original_formula_weight         1986.26
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1830.1(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7133609
_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.
;
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
Br01 Br 1.01320(8) 0.42762(5) 0.61452(4) 0.0594(3) Uani 1 1 d . . . . .
Zn02 Zn 0.81487(8) 0.29448(5) 0.57686(3) 0.0445(2) Uani 1 1 d . . . . .
Br03 Br 0.93673(13) 0.13043(7) 0.55190(4) 0.0895(3) Uani 1 1 d . . . . .
S004 S 0.6199(3) 0.48084(14) 0.79231(10) 0.0698(5) Uani 1 1 d . . . . .
N005 N 0.6422(6) 0.3416(3) 0.4986(2) 0.0386(11) Uani 1 1 d . . . . .
N006 N 0.5764(6) 0.3023(3) 0.6290(2) 0.0386(11) Uani 1 1 d . . . . .
N007 N 0.4348(6) 0.3110(4) 0.5816(2) 0.0454(12) Uani 1 1 d D . . . .
C008 C 0.4737(8) 0.3443(4) 0.5143(3) 0.0407(13) Uani 1 1 d . . . . .
C009 C 0.5472(8) 0.2929(5) 0.6946(3) 0.0454(14) Uani 1 1 d . . . . .
C00A C 0.6841(8) 0.3723(5) 0.4332(3) 0.0497(16) Uani 1 1 d . . . . .
H00C H 0.801808 0.371132 0.421334 0.060 Uiso 1 1 calc R U . . .
C00B C 0.7062(7) 0.2842(5) 0.7423(3) 0.0464(15) Uani 1 1 d . . . . .
C00C C 0.3874(9) 0.4069(5) 0.4023(3) 0.0517(16) Uani 1 1 d . . . . .
H00D H 0.301249 0.429274 0.369684 0.062 Uiso 1 1 calc R U . . .
C00D C 0.5606(9) 0.4043(5) 0.3852(3) 0.0510(15) Uani 1 1 d . . . . .
H00E H 0.592912 0.424464 0.340880 0.061 Uiso 1 1 calc R U . . .
C00E C 0.3408(8) 0.3763(5) 0.4678(3) 0.0529(16) Uani 1 1 d . . . . .
H00F H 0.223616 0.377115 0.480359 0.063 Uiso 1 1 calc R U . . .
C00F C 0.8151(8) 0.1961(5) 0.7373(3) 0.0550(17) Uani 1 1 d . . . . .
H00G H 0.788486 0.144406 0.703931 0.066 Uiso 1 1 calc R U . . .
C00G C 0.3664(8) 0.2880(5) 0.7228(3) 0.0572(17) Uani 1 1 d . . . . .
H00H H 0.308002 0.354883 0.715248 0.086 Uiso 1 1 calc R U . . .
H00I H 0.375466 0.273208 0.771950 0.086 Uiso 1 1 calc R U . . .
H00J H 0.299726 0.232919 0.699391 0.086 Uiso 1 1 calc R U . . .
C00H C 0.7475(8) 0.3632(5) 0.7915(3) 0.0522(16) Uani 1 1 d . . . . .
C00I C 0.9631(9) 0.1845(6) 0.7817(4) 0.069(2) Uani 1 1 d . . . . .
H00K H 1.036144 0.125594 0.778044 0.082 Uiso 1 1 calc R U . . .
C00J C 0.8978(9) 0.3522(6) 0.8360(4) 0.0665(19) Uani 1 1 d . . . . .
H00L H 0.928309 0.404877 0.868264 0.080 Uiso 1 1 calc R U . . .
C00K C 1.0002(10) 0.2615(7) 0.8311(4) 0.072(2) Uani 1 1 d . . . . .
H00M H 1.096599 0.252347 0.862126 0.087 Uiso 1 1 calc R U . . .
C00L C 0.5765(12) 0.4966(6) 0.8845(4) 0.078(2) Uani 1 1 d . . . . .
H00N H 0.687988 0.495944 0.911199 0.094 Uiso 1 1 calc R U . . .
H00O H 0.521881 0.565242 0.891325 0.094 Uiso 1 1 calc R U . . .
C00M C 0.4588(14) 0.4118(7) 0.9123(5) 0.101(3) Uani 1 1 d . . . . .
H00P H 0.348170 0.411772 0.886088 0.152 Uiso 1 1 calc R U . . .
H00Q H 0.438531 0.425621 0.960542 0.152 Uiso 1 1 calc R U . . .
H00R H 0.514674 0.343892 0.907966 0.152 Uiso 1 1 calc R U . . .
H1N H 0.326(5) 0.327(5) 0.595(4) 0.08(2) Uiso 1 1 d 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'
Br Br -0.2901 2.4595 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
N005 Zn02 N006 78.31(17) . . ?
N005 Zn02 Br03 110.90(12) . . ?
N006 Zn02 Br03 119.76(13) . . ?
N005 Zn02 Br01 113.70(13) . . ?
N006 Zn02 Br01 111.88(13) . . ?
Br03 Zn02 Br01 116.41(4) . . ?
C00H S004 C00L 102.8(3) . . ?
C008 N005 C00A 117.7(5) . . ?
C008 N005 Zn02 115.9(4) . . ?
C00A N005 Zn02 126.4(4) . . ?
C009 N006 N007 119.2(5) . . ?
C009 N006 Zn02 130.0(4) . . ?
N007 N006 Zn02 110.6(3) . . ?
N006 N007 C008 116.3(5) . . ?
N005 C008 C00E 123.2(5) . . ?
N005 C008 N007 116.3(5) . . ?
C00E C008 N007 120.6(5) . . ?
N006 C009 C00B 116.1(5) . . ?
N006 C009 C00G 123.5(5) . . ?
C00B C009 C00G 120.4(5) . . ?
C00D C00A N005 122.1(6) . . ?
C00F C00B C00H 119.9(6) . . ?
C00F C00B C009 119.1(6) . . ?
C00H C00B C009 121.0(5) . . ?
C00D C00C C00E 119.9(6) . . ?
C00A C00D C00C 119.4(6) . . ?
C00C C00E C008 117.7(6) . . ?
C00I C00F C00B 120.7(7) . . ?
C00B C00H C00J 119.6(6) . . ?
C00B C00H S004 119.7(5) . . ?
C00J C00H S004 120.5(6) . . ?
C00K C00I C00F 119.0(7) . . ?
C00K C00J C00H 118.9(7) . . ?
C00I C00K C00J 121.9(7) . . ?
C00M C00L S004 113.5(6) . . ?
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
Br01 Zn02 2.3470(10) . ?
Zn02 N005 2.039(5) . ?
Zn02 N006 2.103(4) . ?
Zn02 Br03 2.3224(11) . ?
S004 C00H 1.771(7) . ?
S004 C00L 1.822(7) . ?
N005 C008 1.325(7) . ?
N005 C00A 1.361(7) . ?
N006 C009 1.292(7) . ?
N006 N007 1.381(7) . ?
N007 C008 1.401(7) . ?
C008 C00E 1.377(9) . ?
C009 C00B 1.487(8) . ?
C009 C00G 1.495(8) . ?
C00A C00D 1.348(9) . ?
C00B C00F 1.389(8) . ?
C00B C00H 1.397(9) . ?
C00C C00D 1.366(9) . ?
C00C C00E 1.373(9) . ?
C00F C00I 1.388(10) . ?
C00H C00J 1.403(9) . ?
C00I C00K 1.378(11) . ?
C00J C00K 1.388(10) . ?
C00L C00M 1.504(11) . ?
