#------------------------------------------------------------------------------
#$Date: 2025-08-20 21:19:29 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301836 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/29/4302903.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_4302903
loop_
_publ_author_name
'Shih-Mao Ho'
'Ching-Sheng Hsiao'
'Amitabha Datta'
'Chen-Hsiung Hung'
'Ling-Chueh Chang'
'Ting-Yu Lee'
'Jui-Hsien Huang'
_publ_section_title
;
Monomeric, Dimeric, and Trimeric Calcium Compounds Containing Substituted
Pyrrolyl and Ketiminate Ligands: Synthesis and Structural Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8004
_journal_page_last               8011
_journal_paper_doi               10.1021/ic900265c
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C53 H92 Ca2 N4 O2 Si4'
_chemical_formula_sum            'C53 H92 Ca2 N4 O2 Si4'
_chemical_formula_weight         1009.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.253(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8253(9)
_cell_length_b                   17.5332(13)
_cell_length_c                   15.4155(12)
_cell_measurement_temperature    273(2)
_cell_volume                     3052.4(4)
_computing_cell_refinement       'SAINT v6.280a (Bruker, 2004)'
_computing_data_collection       'APEX2 v1.0-22 (Bruker, 2004)'
_computing_data_reduction        'SAINT v6.280a (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL 5.1'
_computing_publication_material  'SHELXTL 5.1'
_computing_structure_refinement  'SHELXTL 5.1'
_computing_structure_solution    'SHELXTL 5.1 (Sheldrick, 1998)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       ω
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45537
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         7361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0363
_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)+(0.0437P)²+0.9126P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                5670
_reflns_number_total             7361
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900265c_si_001_3.cif
_cod_data_source_block           Cpd3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4302903
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.22217(16) -0.00667(10) -0.22236(12) 0.0417(4) Uani 1 1 d . . .
H1A H -0.1998 -0.0591 -0.2243 0.063 Uiso 1 1 calc R . .
H1B H -0.2540 0.0123 -0.2832 0.063 Uiso 1 1 calc R . .
H1C H -0.2810 -0.0027 -0.1910 0.063 Uiso 1 1 calc R . .
C2 C -0.11525(13) 0.03951(8) -0.17324(10) 0.0258(3) Uani 1 1 d . . .
C3 C -0.07900(13) 0.09749(9) -0.21661(10) 0.0264(3) Uani 1 1 d . . .
H3 H -0.1245 0.1054 -0.2764 0.032 Uiso 1 1 calc R . .
C4 C 0.02003(13) 0.14899(8) -0.18366(10) 0.0239(3) Uani 1 1 d . . .
C5 C 0.05616(15) 0.18938(10) -0.25771(10) 0.0321(4) Uani 1 1 d . . .
H5A H -0.0046 0.2248 -0.2880 0.048 Uiso 1 1 calc R . .
H5B H 0.0671 0.1526 -0.3007 0.048 Uiso 1 1 calc R . .
H5C H 0.1289 0.2164 -0.2315 0.048 Uiso 1 1 calc R . .
C6 C 0.16870(12) 0.21374(8) -0.07037(9) 0.0233(3) Uani 1 1 d . . .
C7 C 0.14659(14) 0.29261(9) -0.07264(11) 0.0287(3) Uani 1 1 d . . .
C8 C 0.24344(16) 0.34111(9) -0.04046(12) 0.0371(4) Uani 1 1 d . . .
H8 H 0.2307 0.3935 -0.0407 0.044 Uiso 1 1 calc R . .
C9 C 0.35720(15) 0.31381(10) -0.00848(12) 0.0386(4) Uani 1 1 d . . .
H9 H 0.4204 0.3475 0.0113 0.046 Uiso 1 1 calc R . .
C10 C 0.37715(14) 0.23632(10) -0.00588(12) 0.0352(4) Uani 1 1 d . . .
H10 H 0.4542 0.2180 0.0161 0.042 Uiso 1 1 calc R . .
C11 C 0.28392(13) 0.18492(9) -0.03566(10) 0.0271(3) Uani 1 1 d . . .
C12 C 0.02266(15) 0.32587(9) -0.10777(12) 0.0354(4) Uani 1 1 d . . .
H12 H -0.0316 0.2845 -0.1360 0.042 Uiso 1 1 calc R . .
C13 C 0.01493(19) 0.38756(12) -0.17998(14) 0.0526(5) Uani 1 1 d . . .
H13A H -0.0659 0.4035 -0.2049 0.079 Uiso 1 1 calc R . .
H13B H 0.0432 0.3673 -0.2276 0.079 Uiso 1 1 calc R . .
H13C H 0.0627 0.4305 -0.1527 0.079 Uiso 1 1 calc R . .
C14 C -0.0177(2) 0.35837(13) -0.03076(15) 0.0543(5) Uani 1 1 d . . .
H14A H -0.0166 0.3189 0.0127 0.081 Uiso 1 1 calc R . .
H14B H -0.0968 0.3779 -0.0545 0.081 Uiso 1 1 calc R . .
H14C H 0.0346 0.3988 -0.0017 0.081 Uiso 1 1 calc R . .
C15 C 0.30774(15) 0.09966(9) -0.03361(12) 0.0350(4) Uani 1 1 d . . .
H15 H 0.2354 0.0737 -0.0311 0.042 Uiso 1 1 calc R . .
C16 C 0.3327(2) 0.07416(14) -0.11989(15) 0.0652(7) Uani 1 1 d . . .
H16A H 0.2668 0.0871 -0.1713 0.098 Uiso 1 1 calc R . .
H16B H 0.3446 0.0199 -0.1182 0.098 Uiso 1 1 calc R . .
H16C H 0.4027 0.0992 -0.1249 0.098 Uiso 1 1 calc R . .
C17 C 0.40712(16) 0.07434(10) 0.04905(13) 0.0408(4) Uani 1 1 d . . .
H17A H 0.4812 0.0937 0.0448 0.061 Uiso 1 1 calc R . .
H17B H 0.4100 0.0196 0.0514 0.061 Uiso 1 1 calc R . .
H17C H 0.3929 0.0937 0.1031 0.061 Uiso 1 1 calc R . .
C18 C 0.1079(2) 0.18921(14) 0.32506(13) 0.0557(6) Uani 1 1 d . . .
H18A H 0.0405 0.1972 0.3466 0.083 Uiso 1 1 calc R . .
H18B H 0.1763 0.2128 0.3661 0.083 Uiso 1 1 calc R . .
H18C H 0.1218 0.1355 0.3218 0.083 Uiso 1 1 calc R . .
C19 C 0.0468(2) 0.33546(12) 0.22547(15) 0.0553(6) Uani 1 1 d . . .
H19A H 0.0330 0.3620 0.1688 0.083 Uiso 1 1 calc R . .
H19B H 0.1133 0.3579 0.2699 0.083 Uiso 1 1 calc R . .
H19C H -0.0221 0.3392 0.2460 0.083 Uiso 1 1 calc R . .
C20 C 0.22286(15) 0.23082(11) 0.18211(13) 0.0393(4) Uani 1 1 d . . .
H20A H 0.2428 0.1791 0.1722 0.059 Uiso 1 1 calc R . .
H20B H 0.2839 0.2522 0.2319 0.059 Uiso 1 1 calc R . .
H20C H 0.2157 0.2603 0.1283 0.059 Uiso 1 1 calc R . .
C21 C -0.24666(17) 0.28040(12) 0.09075(14) 0.0473(5) Uani 1 1 d . . .
H21A H -0.2204 0.3100 0.1455 0.071 Uiso 1 1 calc R . .
H21B H -0.3309 0.2738 0.0746 0.071 Uiso 1 1 calc R . .
H21C H -0.2266 0.3065 0.0426 0.071 Uiso 1 1 calc R . .
C22 C -0.2213(2) 0.13738(15) 0.20064(15) 0.0592(6) Uani 1 1 d . . .
H22A H -0.1888 0.0868 0.2105 0.089 Uiso 1 1 calc R . .
H22B H -0.3062 0.1345 0.1825 0.089 Uiso 1 1 calc R . .
H22C H -0.1940 0.1663 0.2558 0.089 Uiso 1 1 calc R . .
C23 C -0.24137(16) 0.12847(12) 0.00165(13) 0.0429(4) Uani 1 1 d . . .
H23A H -0.2165 0.1496 -0.0471 0.064 Uiso 1 1 calc R . .
H23B H -0.3261 0.1310 -0.0134 0.064 Uiso 1 1 calc R . .
H23C H -0.2163 0.0763 0.0110 0.064 Uiso 1 1 calc R . .
Ca1 Ca 0.01822(3) 0.102055(16) 0.027186(19) 0.02373(8) Uani 1 1 d . . .
N1 N 0.07209(10) 0.16016(7) -0.09780(8) 0.0222(2) Uani 1 1 d . . .
N2 N -0.02501(11) 0.18571(7) 0.12708(8) 0.0269(3) Uani 1 1 d . . .
O1 O -0.06378(9) 0.01782(6) -0.08861(7) 0.0267(2) Uani 1 1 d . . .
Si1 Si 0.07882(4) 0.23246(3) 0.20939(3) 0.02932(11) Uani 1 1 d . . .
Si2 Si -0.17269(4) 0.18492(3) 0.10943(3) 0.03189(11) Uani 1 1 d . . .
C24 C 0.2877(5) 0.5256(3) -0.1318(3) 0.0772(17) Uani 0.50 1 d P A 1
H24A H 0.2940 0.5171 -0.1918 0.116 Uiso 0.50 1 calc PR A 1
H24B H 0.2616 0.5769 -0.1273 0.116 Uiso 0.50 1 calc PR A 1
H24C H 0.2315 0.4904 -0.1203 0.116 Uiso 0.50 1 calc PR A 1
C25 C 0.3973(2) 0.51446(12) -0.06845(19) 0.0641(6) Uani 1 1 d . . .
H25A H 0.3279 0.5244 -0.1146 0.077 Uiso 0.50 1 calc PR A 2
C26 C 0.4019(2) 0.52486(12) 0.02175(19) 0.0649(7) Uani 1 1 d . A .
H26A H 0.3350 0.5416 0.0362 0.078 Uiso 1 1 calc R . .
C27 C 0.5033(3) 0.51068(12) 0.08895(19) 0.0664(7) Uani 1 1 d . . .
H27A H 0.5058 0.5180 0.1493 0.080 Uiso 1 1 calc R A .
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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 C2 C3 125.65(13) . . ?
O1 C2 C1 114.50(14) . . ?
C3 C2 C1 119.85(14) . . ?
C2 C3 C4 129.58(13) . . ?
N1 C4 C3 122.81(13) . . ?
N1 C4 C5 123.05(14) . . ?
C3 C4 C5 114.13(13) . . ?
C11 C6 C7 121.10(13) . . ?
C11 C6 N1 118.21(13) . . ?
C7 C6 N1 120.54(13) . . ?
C8 C7 C6 117.64(14) . . ?
C8 C7 C12 119.75(14) . . ?
C6 C7 C12 122.61(14) . . ?
C9 C8 C7 121.91(16) . . ?
C8 C9 C10 119.67(15) . . ?
C9 C10 C11 121.12(15) . . ?
C10 C11 C6 118.52(15) . . ?
C10 C11 C15 120.41(14) . . ?
C6 C11 C15 121.03(13) . . ?
C14 C12 C7 111.08(15) . . ?
C14 C12 C13 109.77(16) . . ?
C7 C12 C13 111.87(15) . . ?
C16 C15 C11 110.84(16) . . ?
C16 C15 C17 110.27(15) . . ?
C11 C15 C17 113.38(14) . . ?
N2 Ca1 O1 143.75(4) . . ?
N2 Ca1 O1 112.30(4) . 3 ?
O1 Ca1 O1 74.11(4) . 3 ?
N2 Ca1 N1 115.37(4) . . ?
O1 Ca1 N1 78.62(4) . . ?
O1 Ca1 N1 128.72(4) 3 . ?
N2 Ca1 Ca1 137.97(4) . 3 ?
O1 Ca1 Ca1 37.09(3) . 3 ?
O1 Ca1 Ca1 37.01(3) 3 3 ?
N1 Ca1 Ca1 105.59(3) . 3 ?
C4 N1 C6 119.47(12) . . ?
C4 N1 Ca1 126.12(10) . . ?
C6 N1 Ca1 114.36(8) . . ?
Si2 N2 Si1 127.69(8) . . ?
Si2 N2 Ca1 108.25(6) . . ?
Si1 N2 Ca1 123.84(7) . . ?
C2 O1 Ca1 123.13(9) . . ?
C2 O1 Ca1 130.68(9) . 3 ?
Ca1 O1 Ca1 105.89(4) . 3 ?
N2 Si1 C20 109.28(7) . . ?
N2 Si1 C18 113.89(8) . . ?
C20 Si1 C18 106.58(10) . . ?
N2 Si1 C19 115.80(8) . . ?
C20 Si1 C19 106.08(10) . . ?
C18 Si1 C19 104.55(10) . . ?
N2 Si2 C22 114.71(9) . . ?
N2 Si2 C21 115.60(8) . . ?
C22 Si2 C21 106.33(11) . . ?
N2 Si2 C23 107.43(7) . . ?
C22 Si2 C23 106.22(10) . . ?
C21 Si2 C23 105.83(9) . . ?
C27 C25 C24 124.5(4) 3_665 . ?
C27 C25 C26 119.4(3) 3_665 . ?
C24 C25 C26 116.0(4) . . ?
C27 C26 C25 120.3(2) . . ?
C26 C27 C25 120.4(3) . 3_665 ?
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 C2 1.503(2) . ?
C2 O1 1.3215(17) . ?
C2 C3 1.354(2) . ?
C3 C4 1.446(2) . ?
C4 N1 1.2984(18) . ?
C4 C5 1.509(2) . ?
C6 C11 1.402(2) . ?
C6 C7 1.406(2) . ?
C6 N1 1.4422(18) . ?
C7 C8 1.394(2) . ?
C7 C12 1.520(2) . ?
C8 C9 1.374(2) . ?
C9 C10 1.377(2) . ?
C10 C11 1.392(2) . ?
C11 C15 1.520(2) . ?
C12 C14 1.516(3) . ?
C12 C13 1.535(2) . ?
C15 C16 1.513(3) . ?
C15 C17 1.521(2) . ?
C18 Si1 1.873(2) . ?
C19 Si1 1.876(2) . ?
C20 Si1 1.8719(19) . ?
C21 Si2 1.871(2) . ?
C22 Si2 1.866(2) . ?
C23 Si2 1.8971(18) . ?
Ca1 N2 2.2915(13) . ?
Ca1 O1 2.2981(10) . ?
Ca1 O1 2.3025(10) 3 ?
Ca1 N1 2.4257(12) . ?
Ca1 Ca1 3.6717(6) 3 ?
N2 Si2 1.6858(13) . ?
N2 Si1 1.6927(13) . ?
O1 Ca1 2.3025(10) 3 ?
C24 C25 1.386(6) . ?
C25 C27 1.376(4) 3_665 ?
C25 C26 1.388(4) . ?
C26 C27 1.355(4) . ?
C27 C25 1.376(4) 3_665 ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139126935
