Carbon-sulphur cross coupling reactions catalyzed by nickel-based coordination polymers based on metalloligands.
Kumar, Gulshan; Hussain, Firasat; Gupta, Rajeev; Dalton transactions (Cambridge, England : 2003) 46 (2017) 15023–15031; doi:10.1039/c7dt02064c

data_7702134
_publ_section_title
;
 Carbon-sulphur cross coupling reactions catalyzed by nickel-based
 coordination polymers based on metalloligands.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15023
_journal_page_last               15031
_journal_paper_doi               10.1039/c7dt02064c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         '0.33(C126 H114 Co3 N18 Ni6 O60), 4(H2 O)'
_chemical_formula_sum            'C42 H46 Co N6 Ni2 O24'
_chemical_formula_weight         1195.20
_space_group_crystal_system      hexagonal
_space_group_IT_number           180
_space_group_name_Hall           'P 62 2 (0 0 4)'
_space_group_name_H-M_alt        'P 62 2 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-10-01 deposited with the CCDC.
2017-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   27.857(2)
_cell_length_b                   27.857(2)
_cell_length_c                   10.0365(7)
_cell_measurement_reflns_used    1197
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.5710
_cell_measurement_theta_min      3.6610
_cell_volume                     6745.0(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1768
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            67475
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.883
_exptl_crystal_description       needle
_exptl_crystal_F_000             1845
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 963 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4121
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0543
_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/[\s^2^(Fo^2^)+(0.0488P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3255
_reflns_number_total             4121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02064c2.cif
_cod_data_source_block           1ni_sq
_cod_original_cell_volume        6745.2(11)
_cod_original_sg_symbol_Hall     'P 62 2c (0 0 1)'
_cod_database_code               7702134
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.881
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, All H(H,H) groups, All C(H) groups
2. Restrained distances
 O1W-H1WA = O4-H4
 0.82 with sigma of 0.02
 O1W-H1WB = O6-H6A
 0.82 with sigma of 0.02
 O5-H5A = O5-H5B
 0.82 with sigma of 0.02
 O1W-H1WA = O4-H4
 1.39 with sigma of 0.02
 O1W-H1WB = O6-H6A
 1.39 with sigma of 0.02
 O5-H5A = O5-H5B
 1.39 with sigma of 0.02
3.a Everything fixed:
 H1WA, H1WB, H5A, H5B, H6A(H4)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C9(H9), C10(H10)
;
_shelx_res_checksum              36867
_shelx_fab_checksum              15076
_olex2_submission_special_instructions 'No special instructions were received'